CN100554484C - Fe based amorphous nano dusty spray and argon gas atomization production thereof - Google Patents
Fe based amorphous nano dusty spray and argon gas atomization production thereof Download PDFInfo
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- CN100554484C CN100554484C CNB2007100653597A CN200710065359A CN100554484C CN 100554484 C CN100554484 C CN 100554484C CN B2007100653597 A CNB2007100653597 A CN B2007100653597A CN 200710065359 A CN200710065359 A CN 200710065359A CN 100554484 C CN100554484 C CN 100554484C
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Abstract
A kind of Fe based amorphous nano dusty spray and argon gas atomization production thereof belong to amorphous nano-crystalline powder technology field.Fe based amorphous nano dusty spray is on the basis of Fe-TM-B amorphous alloys, and the weight percentage of composition is: 8～15%wt Cr, 8～16%wtNi, 2.8～5.7%wt Si, 2.8～5%wt B, 2～8%wt W, 2～8%wt Mo, 0.5～1%wt Co, 1～4%wt Al surplus are Fe.Preparation technology's flow process is: composition proportion---vacuum melting---atomizing---powder sieving.The present invention has successfully prepared the Fe amorphous nano-crystalline dusty spray that not only contains non-crystal structure but also contain nanocrystalline structure by the argon gas atomising method, and this powder has good flowability and stability.
Description
Technical field
The present invention relates to amorphous nano-crystalline powder technology field, particularly relate to a kind of Fe based amorphous nano dusty spray and argon gas atomization production thereof.
Background technology
The amorphous-nano-crystalline material has the performance more unique and more excellent than traditional material, is rising type material.But in practice, so far, these materials are not still also applied on a large scale, and its principal element is that its preparation process is difficult to control, and its application mainly is limited in low dimensions such as strip, filament, powder in shape.Comparatively speaking, the preparation process of amorphous nanocrystalline coating just realizes than being easier to, and in numerous methods that prepare coating, hot-spraying techniques is a kind of technology that has competitive power, also is very promising technology simultaneously.Utilize hot-spraying techniques to obtain the amorphous nano crystallization that the amorphous-nano-crystalline compound coating is decided by dusty spray to a great extent.Can therefore obtain good stability, mobile strong amorphous nano-crystalline composite powder have just become to obtain an important factor of amorphous-nano-crystalline compound coating.
The preparation method of powder is a lot, and the aerosolization energy consumption is little, and is free from environmental pollution, powder purity height, and good sphericity, and powder characteristics is controlled has become the main direction of high-performance spray powdered preparation technical development in the world in this year.Because of the oxygen level in the dusty spray has very big influence for the raising of spraying process powder sending quantity and the performance raising of coating; so vacuum aerosolization technology becomes the mainstream technology for preparing the high-performance spray powder this year; its powder process principle is as follows; metal or alloy melts in crucible under the vacuum state protection of inert gas and reaches after certain temperature of superheat; push plunger rod aside; the metal or alloy liquation atomizing nozzle of flowing through downwards; meet high pressure draft; the direct impact grinding metal or alloy of this air-flow solution becomes drop and cools off the fine particle that these drops become partly to solidify, and these particles are condensed into microcrystal powder in free flight.
The Fe base noncrystal alloy is as a kind of novel material, have the anti-corrosion of excellence, wear-resisting, performances such as high intensity and toughness more and more are subjected to people's extensive attention, its tensile strength is at room temperature up to 1433MPa, be 2.27 times of conventional iron crystal tensile strength (630MPa) approximately, compressive strength and Vickers' hardness reach 3800MPa and 1360HV respectively, and fracture toughness property has reached 1.6MPam
1/2But the limitations restrict of large block amorphous preparation process its practical application, utilize hot-spraying techniques to can solve this problem.People such as Wang Cuiling and Fan Zishuan just utilizes hypersonic flame spraying and atmospheric plasma technology successfully to prepare Fe based amorphous-nano-crystalline compound coating respectively, enlarge the range of application of amorphous-nano-crystalline alloy, and utilized the amorphous-nano-crystalline compound coating of hot-spraying techniques preparation to keep the good wear and corrosion behavior of amorphous alloy.
Seek out the amorphous nano crystallization that amorphous nanocrystalline coating is decided by dusty spray to a great extent.J.G.Zhang and Y.J.Liu etc. utilize chemical vapour deposition and mechanical alloying method to prepare the Fe based amorphous alloy powder respectively; People such as Yoon B.Kim and E.Y.Kang utilize aerosolization technology successfully to prepare Fe base amorphous powder.Though the acquisition by different explained hereafter method successes the Fe based amorphous alloy powder, but major part is that its good magnetic property is studied, its application in thermospray is not studied, and above-mentioned prepared powder all is single amorphous powders, seeking out the powder that contains nanocrystalline crystal grain must handle through crystallization, and all there is certain limitation in too high it is used of the complicacy of technology and cost.The present invention proposes directly to obtain Fe based amorphous-nano-crystalline composite powder by to alloying constituent and control of process parameters.
Summary of the invention
The object of the present invention is to provide a kind of Fe based amorphous nano dusty spray and argon gas atomization production thereof, how to have solved by to the amorphous nano crystallization of dusty spray and more simply obtain the problem of amorphous nanocrystalline coating.
The present invention proposes to adopt the argon gas atomising method directly to prepare Fe based amorphous nano powder, some alloy ore deposits of selecting Fe for use are as raw material, calculate per-cent by composition and carry out the melting atomizing, sieving out varigrained dusty spray by the requirement of different spraying coating process after preparing the Fe based powders.
Fe based amorphous nano dusty spray of the present invention is on the basis of Fe-TM-B (TM=IV～VIII transiting group metal elements) amorphous alloys, the weight percentage of composition is: 8～15%wt Cr, 8～16%wtNi, 2.8～5.7%wtSi, 2.8～5%wt B, 2～8%wt W, 2～8%wt Mo, 0.5～1%wt Co, 1～4%wt Al surplus are Fe,, carry out the melting and the vacuum atomizing of mother alloy.
The proportioning of powder composition is according to three fundamental principles that form amorphous alloy, and selecting the aerosolization production technique for use then is to obtain the sphericity height, the dusty spray of good fluidity.
The present invention adopts aerosolization technology as the method for preparing powder, and technical process is: composition proportion-vacuum melting-atomizing-powder sieving.Processing parameter is: melting vacuum 1 * 10
-4～1 * 10
-2Pa, 1500～1800 ℃ of smelting temperatures, atomizing pressure 2.5～4MPa, atomizing medium: argon gas.
The invention has the advantages that according to three compositions of passing the choose reasonable alloy in principle that obtain bulk amorphous alloys, utilize argon gas atomizing rapid cooling method to prepare Fe based amorphous nano dusty spray, thereby the sphericity of the powder of feasible preparation is very good, powder size distributes rationally, and has good flowability.
Description of drawings
Fig. 1 is the pattern photo (2500 *) of Fe base dusty spray
Fig. 2 is the X ray diffracting spectrum of Fe base dusty spray
Fig. 3 is the TEM shape appearance figure of Fe base dusty spray
Fig. 4 is the micro-area diffraction style of Fe base dusty spray
Fig. 5 be Fe base dusty spray differential thermal analysis (DSC) curve
Fig. 6 is the particle size distribution figure of Fe base dusty spray
Embodiment
The composition of Fe Quito element amorphous nano-crystalline powdered alloy is by weight percentage: 1%C, 4.5%Si, 2.5%B, 18%Cr, 8%Ni, 6%W 4%Mo, remaining be Fe, master alloy melting in vacuum induction melting furnace, the parameter of melting is: melting vacuum 5X10
-1Pa, 1600 ℃ of Heating temperatures, frequency: 4kHz power input: 30KW.
Embodiment 2
The composition of Fe Quito element amorphous nano-crystalline powdered alloy is by weight percentage: 6%Si, 4%B, 10%Zr, 6%Ni, 4%Al, remaining be Fe, master alloy melting in vacuum induction melting furnace, the parameter of melting is: melting vacuum 5X10
-1Pa, 1600 ℃ of Heating temperatures, frequency: 4kHz, power input: 30KW.
Embodiment 3
The composition of Fe Quito element amorphous nano-crystalline powder is by weight percentage: 4.5%Si, 2.5%B, 8%Cr, 6%Ni, 6%W, 8%Mo remainder be Fe, master alloy melting in vacuum induction melting furnace, the parameter of melting is: melting vacuum 5X10
-1Pa, 1600 ℃ of Heating temperatures, frequency: 4kHz, power input: 30KW.
The composition of Fe Quito element amorphous nano-crystalline powder is by weight percentage: 5.8%Si, 2.7%B, 15%Cr, 15%Ni, 4%W, 6%Mo, 1%Co, 2%Al remainder be Fe, master alloy melting in vacuum induction melting furnace, the parameter of melting is: melting vacuum 5X10
-1Pa, 1600 ℃ of Heating temperatures, frequency: 4kHz, power input: 30KW.
Select embodiment 4 to do the powder property analysis.
The crystalline structure of dusty spray
Fig. 1 is the pattern photo of the Fe base dusty spray (325 order) of preparation, and all spherical in shape or elliposoidal of prepared as can be seen powder, and very smooth of surface have good flowability.Fig. 2 is the X ray diffracting spectrum of Fe base dusty spray, as can be seen in the powder except containing amorphous, also contain Al
0.3Fe
3Si
0.7And Ni
4B
3Phase, Al
0.3Fe
3Si
0.7Average crystal grain is 36.45nm, Ni
4B
3Average crystal grain is 65.68nm, and as seen, the size of crystal grain below 100nm, all is nanocrystalline all, illustrates that prepared dusty spray is the amorphous manocrystalline powders.Adopt alloying constituent proportioning of the present invention and producing and manufacturing technique to prepare Fe based amorphous nano compound coating.
The heterogeneous microstructure of coating
With transmission electron microscope observing the heterogeneous microstructure of coating, the results are shown in accompanying drawing 3.Therefrom as can be seen:, it is not homogeneous very that the interior microscopic of powder is organized contrast, illustrate that prepared powder particle structure not exclusively is a non-crystal structure, the disperse precipitated phase that a spot of nanoscale is arranged, measure the size of these polycrystalline compositions, measure its distribution of sizes between 10～100nm, identical substantially with the halfwidth of the diffraction peak of using the X diffraction through the grain-size that the Scherrer formula calculates.The micro-area diffraction style (see figure 5) of respective regions has also shown in the prepared Fe base dusty spray also contained crystalline material except containing amorphous, and crystalline material is a nano-scale, as seen adopts alloying constituent proportioning of the present invention and producing and manufacturing technique to prepare Fe based amorphous nano compound coating.
The thermostability of powder
With the DSC curve of having measured powder on the NETZSCH STA 409C thermal analyzer, selecting argon gas for use is protective gas, and the flow velocity of argon gas is 20ml/min, and heat-up rate is 30.0K/min, and the scope of intensification is 25 ℃ to 800 ℃.Experimental data is seen accompanying drawing 6, and therefrom as can be seen: initial crystallization temperature is about 570.8 ℃, and this shows that 570.8 ℃ of following coatings be stable, crystallization process can not take place.T=90.1 ℃ of supercooling liquid phase region Δ before the amorphous structure phase crystallization in the powder shows that prepared Fe based powders has stronger amorphous formation ability.The prepared Fe based amorphous nano dusty spray of the present invention has very high thermostability.
The size-grade distribution of powder
With LMS-30 laser particle size distribution recognizer negative 325 purpose dusty spraies have been carried out sreen analysis, dispersion medium is a water, sample solution concentration 798mV, and testing data is seen accompanying drawing 6, therefrom as can be seen, the mean particle size of powder is 21.933 μ m; The powder of globule size between 16.58～32.78 μ m accounts for 81% of powder altogether, the normal distribution that powder is described is narrow, and the ratio that the powder of globule size between 5.03～13.98 μ m and 38.86～54.64 μ m accounts for is respectively 10.64% and 9%, in the size-grade distribution of this explanation powder, containing a certain amount of small-particle and macrobead, is very favourable for forming high fine and close coating in the spraying process.The prepared Fe based amorphous nano powder of the present invention meets the requirement of spraying process very much.
Claims (2)
1, a kind of Fe based amorphous nano dusty spray, it is characterized in that, on the basis of Fe-TM-B amorphous alloys, the weight percentage of composition is: 8～15%wt Cr, 8～16%wt Ni, 2.8～5.7%wt Si, 2.8～5%wt B, 2～8%wt W, 2～8%wt Mo, 0.5～1%wt Co, 1～4%wt Al surplus are Fe; Wherein, TM=IV～VIII transiting group metal elements; The amorphous nano-crystalline dusty spray is meant and contains the dusty spray that non-crystal structure contains nanocrystalline structure again.
2, the described Fe based amorphous nano of a kind of preparation claim 1 dusty spray method,---vacuum melting---atomizing---powder sieving that it is characterized in that technical process is: composition proportion; Processing parameter is: melting vacuum: 1 * 10
-4～1 * 10
-2Pa, smelting temperature: 1500～1800 ℃, atomizing pressure: 2.5～4MPa, atomizing medium: argon gas; The weight percentage of the mother alloy composition of selecting for use is: 8～15%wt Cr, 8～16%wt Ni, 2.8～5.7%wt Si, 2.8～5%wt B, 2～8%wt W, 2～8%wt Mo, 0.5～1%wt Co, 1～4%wt Al surplus are Fe; The amorphous nano-crystalline dusty spray is meant and contains the dusty spray that non-crystal structure contains nanocrystalline structure again.
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