CN105648423B - Method for manufacturing resistance heating wire - Google Patents

Method for manufacturing resistance heating wire Download PDF

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Publication number
CN105648423B
CN105648423B CN201610098477.7A CN201610098477A CN105648423B CN 105648423 B CN105648423 B CN 105648423B CN 201610098477 A CN201610098477 A CN 201610098477A CN 105648423 B CN105648423 B CN 105648423B
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tungsten
heating wire
resistance heating
metal substrate
laser
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CN105648423A (en
Inventor
刘胜
郑晨居
甘志银
郑怀
林栋�
彭庆
陈斌
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Wuhan University WHU
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Wuhan University WHU
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/46Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for heating the substrate
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00Coating starting from inorganic powder
    • C23C24/08Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/10Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
    • C23C24/103Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides

Abstract

The invention discloses a method for manufacturing a resistance heating wire. A tungsten metal substrate, micron-grade tungsten powder and high-emissivity nanometer materials are prepared; the micron-grade tungsten powder and the high-emissivity nanometer materials are added into a polyvinyl alcohol (PVA) water suspension, and the mixture is evenly stirred through a magnetic stirrer; the surface of the tungsten metal substrate is coated with the mixture of the micron-grade tungsten powder and the high-emissivity nanometer materials through an impregnation method, so that a coating is formed; then the mixture of the micron-grade tungsten powder and the high-emissivity nanometer materials is processed through a laser sintering technology, the coating on the surface of the tungsten metal substrate and the tungsten metal substrate are fused, the high-emissivity nanometer materials are integrated into tungsten metal, and a tungsten-based nanometer composite material is formed; afterwards, the tungsten-based nanometer composite material is processed through a laser shot blasting technology; and finally, the tungsten-based nanometer composite material obtained through the method is made into the resistance heating wire. The emissivity of the resistance heating wire manufactured through the method is greatly improved, the stability of the resistance heating wire working at high temperature is remarkably improved, the service life of the resistance heating wire working at high temperature is remarkably prolonged, and the resistance heating wire is suitable for metal organic chemical vapor deposition (MOCVD).

Description

A kind of resistance heating wire production method
Technical field
The invention belongs to resistance heating wire field, it is related to a kind of resistance heating wire production method.
Background technology
Silicon carbide epitaxy, ultraviolet LED extension and other monocrystal materials need high growth temperature environment.Especially carborundum material Material is a kind of high performance artificial material, has the features such as high intensity, high heat conductance, high-wearing feature and corrosion resistance, in aviation The industrial circles such as space flight, automobile, mechano-electronic, chemical industry are widely used, and are described as the material of God's creation by people.Carborundum Anti-wear performance be cast iron, 5-20 times of rubber service life, Mohs' hardness be 9.5 grades, be only second to Buddha's warrior attendant the hardest in the world Stone(10 grades), it is the very promising high-abrasive material of one kind that high rigidity and anti-wear performance determine carborundum, is extensively made at present It is used for abrading glass, pottery, stone material, hard alloy, titanium alloy etc. for abrasive material.But the growth needs temperature of carborundum is 1650 More than degree, the mode of heating adopting at present is the method for sensing heating, but the method for sensing heating is a kind of Electromagnetic Heating, plus The thermal efficiency is not high, and is difficult to accurately on controlling, and equipment design is complicated.And adopt the heating means of resistance wire or piece, at present Because the level of the emissivity of tungsten material is not high, it is heated to more than the 1400 degree difficulties deposited in design.
MOCVD(Metallo-organic compound chemical gaseous phase deposition)It is the wide variety of semi-conducting material means of production, especially It is the equipment as industrialized production, there are the excellent characteristics such as high stability, repeatability and scale, be that one kind has prospect very much Monocrystal material production method.At present, MOCVD(Metallo-organic compound chemical gaseous phase deposition)Main mode of heating is to adopt Resistant heating, this resistance wire is commonly used refractory metal material tungsten and is manufactured, and has fusing point height, resistivity is big, intensity is good, vapour pressure Low advantage.However, the hardness of tungsten is big and crisp, difficulty of processing increases, and common tungsten filament is once occur through applied at elevated temperature again Will become very crisp after crystallization, be hit or easily rupturing in the case of shaking.Under high-temperature work environment, tungsten enters and moulds Property, substantially reduce the life-span of tungsten.Therefore the functional reliability of tungsten filament and life-span are all relatively low, and general tungsten filament needs annual replacing one Secondary, if material and structure design are bad, or even tens hours are accomplished by changing to hundreds of hour, and a tungsten filament is worth number Ten thousand dollars, costly.Average emitted rate due to tungsten may only have 0.04(Smooth tungsten filament), or 0.032-0.35(Aging Tungsten filament), at present 1200 degrees centigrade are only had using tungsten MOCVD wiry operating temperature, can be used for the life of gallium nitride Long, the growth of aluminium nitride to be carried out, need the temperature of MOCVD to reach 1400 degrees centigrade, if the life of silicon nitride to be carried out Long, the higher temperature of needs, even more than 1700 degrees Celsius.So high growth temperature, if do not improve the emissivity of tungsten, tungsten The temperature of body will reach more than 2000 degree, and the working life of tungsten can substantially reduce, the working life of tungsten to be improved it is therefore desirable to Produce a kind of being capable of high emissivity and be capable of the resistance heating wire of steady operation in high temperature environments.
Content of the invention
In order to solve above-mentioned technical problem, the invention provides a kind of resistance heating wire that can be applicable to MOCVD, by inciting somebody to action Tungsten metal substrate and high emissivity nano material are passed through laser sintering technology and are combined, and are then processed using Laser Peening Technology Can get good reliability under hot conditions, emissivity is high, the resistance wire material of life-span length, its concrete scheme is:
A kind of resistance heating wire production method is it is characterised in that comprise the following steps:
(1)Get out tungsten metal substrate, micron order tungsten powder and high emissivity nano material;
(2)Micron order tungsten powder and high emissivity nano material are added in polyvinyl alcohol (PVA) water slurry, and utilizes magnetic Power agitator stirs;
(3)Using infusion process, micron order tungsten powder and high emissivity nano material mixture are coated in tungsten metallic substrate surfaces Form coating;
(4)Micron order tungsten powder and high emissivity nano material mixture are processed using laser sintering technology, makes tungsten Metal Substrate The coating of plate surface and tungsten metal substrate merge, and high emissivity nano material is integrated in tungsten metal, form tungsten base nanometer multiple Condensation material;
(5)Using Laser Peening Technology, described tungsten based nano composite material is processed;
(6)The tungsten based nano composite material of said method gained is made resistance heating wire, that is, completes resistance heating wire's Make.
As improvement, described micron order tungsten powder average diameter is 50 nanometers -5 microns, and described high emissivity nano material is CNT, Graphene or graphene oxide.
As improvement, described polyvinyl alcohol (PVA) water slurry concentration is 3-5%(wt), to obtain more preferable mixing effect Really.
As improvement, described micron order tungsten powder and high emissivity nano material mixture pass through spraying process or brushing method coating Form coating in tungsten metallic substrate surfaces.
As improvement, described employing laser sintering technology processes micron order tungsten powder and high emissivity nano material mixture mistake Journey is to carry out in the glass chamber full of inert gas, to protect sample not oxidized during laser sintered, by controlling The intensity of laser and sweep speed, keep CNT to be solid-state while so that tungsten powder is melted.
As improvement, described is nitrogen using the inert gas during laser sintered, and described laser is nanosecond laser, skin Second laser and the combination of femtosecond laser or three.
As improvement, described Laser Peening Technology adopts the combination of nanosecond laser, picosecond laser and femtosecond laser or three As the energy, constraint intermediary made by BK 7 glass of HI high impact impedance;To protect tungsten base nanometer multiple with thin aluminium foil for sacrificial coatings layer The surface of condensation material.
As improvement, described tungsten metal substrate is tungsten wire.
Be can be used in the MOCVD need long-time hot operation using the resistance heating wire that said method is obtained.
Present invention has the advantages that:
The tungsten based nano composite material resistance heating wire being made using the inventive method, will be occurred frequently by laser sintering technology The rate nano material of penetrating is integrated in common tungsten metal, can greatly improve the emissivity of resistive heater, thus stabilizing it work Make temperature to be obviously improved than traditional resistor silk, and the effectively save energy;Utilize Laser Peening Technology to tungsten base nanometer simultaneously Composite carries out intensive treatment, makes the resistive heater mechanical performance that the present invention makes outclass traditional resistor silk, effectively changes The job stability of kind resistive heater and working life, thus save production cost;With the resistive heater of the present invention as heat The MOCVD in source with materials such as volume production of silicon carbide, and can effectively reduce production cost.
Brief description
Fig. 1 is that the tungsten based nano composite material having sprayed carries out laser sintered schematic diagram;
Fig. 2 is the structural representation of laser sintered rear tungsten based nano composite material;
Fig. 3 carries out the schematic diagram of laser peening for tungsten based nano composite material.
1 micron order tungsten powder, 2 high emissivity nano materials, 3 tungsten metal substrates, 4 tungsten based nano composite materials, 5 laser arteries and veins Punching, 6 BK 7 glass, 7 thin aluminium foils, 8 plasmas, 9 shock waves.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is illustrated.
As shown in drawings, the invention provides a kind of resistance heating wire production method is it is characterised in that include following walking Suddenly:
(1)Get out tungsten metal substrate 3, micron order tungsten powder 1 and high emissivity nano material 2, described micron order tungsten powder 1 is flat All a diameter of 50 nanometers -5 microns;Described high emissivity nano material 2 is CNT, Graphene, graphene oxide are contour Emissivity material, its black body emissivity reaches 90% about;
(2)Micron order tungsten powder 1 and high emissivity nano material 2 are added in polyvinyl alcohol (PVA) water slurry, and utilizes Uniformly, described polyvinyl alcohol (PVA) water slurry concentration is 3-5% to magnetic stirrer(wt), its optium concentration is 4% (wt), to obtain more preferable mixed effect;
(3)As shown in figure 1, micron order tungsten powder 1 and high emissivity nano material 2 mixture are coated in tungsten using infusion process Metal substrate 3 surface forms coating;
(4)As shown in Fig. 2 being mixed using laser sintering technology process micron order tungsten powder 1 and high emissivity nano material 2 Thing, makes the coating on tungsten metal substrate 3 surface and tungsten metal substrate 3 merge, high emissivity nano material 2 is integrated into tungsten metal In, form tungsten based nano composite material 4;Described employing laser sintering technology processes micron order tungsten powder 1 and high emissivity nanometer material Expect that 2 mixture processes are to carry out in the glass chamber full of nitrogen, to protect sample not oxidized during laser sintered, institute State the combination that laser is nanosecond laser, picosecond laser and femtosecond laser or three, the fusing point of tungsten powder is about 3400 degrees Celsius, graphite All more than 3800 degrees Celsius, the fusing point of CNT is about 4200 degrees Celsius to the fusing point of alkene and graphene oxide, therefore can lead to Cross the intensity controlling laser and sweep speed, keep CNT to be solid-state while so that tungsten powder is melted.
(5)As shown in figure 3, being processed to described tungsten based nano composite material 4 using Laser Peening Technology;Described laser Blasting technology adopts the combination of nanosecond laser, picosecond laser and femtosecond laser or three as the energy, the BK 7 of HI high impact impedance Glass 6 is made the transparent covering layer of constraint intermediary;Tungsten based nano composite material 4 is protected for sacrificial coatings layer with thin aluminium foil 7 Surface;Set gradually as thin aluminium foil 7 and BK 7 glass 6 on the surface of tungsten based nano composite material 4, laser pulse 5 passes through conduct BK 7 glass 6 of transparent covering layer, is partially absorbed by the thin aluminium foil 7 as sacrificial coatings;After thin aluminium foil 7 absorbs laser energy Reach gasification temperature, subsequently plasma 8 is formed by laser pulse 5 ionization;Plasma 8 is limited in the nano combined material of tungsten base Between material 4 and BK 7 glass 6;The plasma 8 of high pressure produces shock wave 9, propagates to BK 7 glass 6 and tungsten base is nano combined On material 4, tungsten based nano composite material 4 is made to produce plastic deformation;After laser peening, tungsten based nano composite material 4 produces Raw near surface processing hardening and near surface residual stress, thus improve the mechanical performance of material.
(6)The tungsten based nano composite material 4 of said method gained is made resistance heating wire, that is, completes resistance heating wire's Make.
Described micron order tungsten powder 1 and high emissivity nano material 2 mixture also can be coated in by spraying process or brushing method Tungsten metal substrate 3 surface forms coating.
Be can be used in the MOCVD need long-time hot operation using the resistance heating wire that said method makes.
The right tungsten based nano composite material of resistive heater proposed by the present invention is constituted, by laser sintering technology by high emission The nano material of rate is integrated in common tungsten metal, can greatly improve the emissivity of resistive heater, thus stabilizing it work Make temperature to be obviously improved than traditional resistor silk, and the effectively save energy;Utilize Laser Peening Technology to tungsten base nanometer simultaneously Composite carries out intensive treatment, makes the mechanical performance of the resistive heater of the present invention outclass traditional resistor silk, is effectively improved The job stability of resistive heater and working life, thus save production cost;With the resistive heater of the present invention as thermal source MOCVD can with materials such as volume production of silicon carbide, and effectively reduce production cost.
Described above be merely exemplary for the purpose of the present invention, and nonrestrictive, the reason of those of ordinary skill in the art Solution, in the case of the spirit and scope being limited without departing from claim, can make change, modify according to the disclosure above content Or equivalent, but fall within protection scope of the present invention.

Claims (5)

1. a kind of resistance heating wire production method is it is characterised in that comprise the following steps:
(1)Get out tungsten metal substrate(3), micron order tungsten powder(1)With high emissivity nano material(2), described micron order tungsten powder (1)Average diameter is 50 nanometers -5 microns, described high emissivity nano material(2)For CNT, Graphene or Graphene oxygen Compound;
(2)By micron order tungsten powder(1)With high emissivity nano material(2)Add in polyvinyl alcohol water slurry, and utilize magnetic force Agitator stirs, and described polyvinyl alcohol water slurry concentration is 3-5% wt;
(3)Using infusion process by micron order tungsten powder(1)With high emissivity nano material(2)Mixture is coated in tungsten metal substrate (3)Surface forms coating;
(4)Micron order tungsten powder is processed using laser sintering technology(1)With high emissivity nano material(2)Mixture, makes tungsten metal Substrate(3)The coating on surface and tungsten metal substrate(3)Merge, high emissivity nano material(2)It is integrated in tungsten metal, formed Tungsten based nano composite material(4);
(5)Using Laser Peening Technology to described tungsten based nano composite material(4)Processed;
(6)Tungsten based nano composite material by said method gained(4)Make resistance heating wire, that is, complete the system of resistance heating wire Make.
2. as claimed in claim 1 a kind of resistance heating wire production method it is characterised in that described micron order tungsten powder(1)And height Emissivity nano material(2)Mixture is coated in tungsten metal substrate by spraying process or brushing method(3)Surface forms coating.
3. as claimed in claim 1 a kind of resistance heating wire production method it is characterised in that described Laser Peening Technology adopt The combination of nanosecond laser, picosecond laser and femtosecond laser or three is as the energy, BK 7 glass of HI high impact impedance(6)Constrain Intermediary;With thin aluminium foil(7)To protect tungsten based nano composite material for sacrificial coatings layer(4)Surface.
4. as claimed in claim 1 a kind of resistance heating wire production method it is characterised in that described tungsten metal substrate(3)For tungsten Wire.
5. adopt the resistance heating wire that the arbitrary methods described of Claims 1-4 is obtained it is characterised in that described resistance heating wire For needing in the MOCVD of long-time hot operation.
CN201610098477.7A 2016-02-23 2016-02-23 Method for manufacturing resistance heating wire Active CN105648423B (en)

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