CN105562680B - The method that a kind of high-entropy alloy powder and hot pressed sintering prepare high-entropy alloy coating - Google Patents
The method that a kind of high-entropy alloy powder and hot pressed sintering prepare high-entropy alloy coating Download PDFInfo
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- CN105562680B CN105562680B CN201610001920.4A CN201610001920A CN105562680B CN 105562680 B CN105562680 B CN 105562680B CN 201610001920 A CN201610001920 A CN 201610001920A CN 105562680 B CN105562680 B CN 105562680B
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
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- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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Abstract
The invention discloses a kind of method that high-entropy alloy powder and hot pressed sintering prepare high-entropy alloy coating, the atomic percent of element composition and various elements in the high-entropy alloy powder is：The % of 18~23 %, Zr 18~23 %, Al 18~23, the % of Ti 18~23 %, Ni 18~23, is prepared using mechanical alloying method, and as coating starting powder, T8 steel matrix surface is sintered in using hot-pressing sintering technique, forms described high-entropy alloy coating.The high-entropy alloy coating that the present invention is prepared using hot-pressing sintering technique is fine and close, and imporosity, flawless, microhardness is high, and sea water corrosion resistance can be good, and its processing technology is simple, production cost is low, has a good application prospect.
Description
Technical field
The invention belongs to material technology floating coat preparation field, and in particular to a kind of high-entropy alloy powder and hot pressed sintering system
The method of standby high-entropy alloy coating.
Background technology
Traditional alloy be with iron, copper, magnesium, aluminium, titanium element, it is basic herein using wherein a certain element as matrix
Upper addition a small amount of one or more of metals or nonmetalloid, the alloy material with some properties is obtained with this.So far
Untill the present, actual development and about nearly hundred kinds of alloy system being widely applied.
2004 mid-terms, researcher jump out the development framework of conventional alloys, propose new alloy design concept, i.e., more pivots
High-entropy alloy.It is exactly that multiple element is pivot, five kinds of essential element and more than, wherein the atomic percent of every kind of essential element
Between 5 ~ 35 %, any element turns into essential element on atomic percent not over 50 %.This conjunction
Gold can't form intermetallic compound, form body-centered cubic, face-centered cubic phase, nano junction with simple crystal structure on the contrary
Structure even non crystalline structure.High-entropy alloy has excellent characteristic such as：Intensity and hardness are high, and corrosion resistance and wearability are good.
Mechanical alloying be it is a kind of obtain alloying powder technology of preparing, the gold almost immiscible under many solid-states
Category, makes each constituent element be combined between reaching atom to form alloy by mechanical alloying.In current preparation technology, mechanical alloy
Change method has obtained very big concern due to the characteristics of its is unique and advantage.
In recent years, new high-entropy alloy constantly is designed and studies.But its preparation means mainly uses vacuum arc furnace ignition
Fusion casting, and the preparation means of high-entropy alloy coating focus primarily upon plasma agglomeration, thermal spraying skill, electric spark deposition, Supersonic
The technology such as fast flame-spraying and pulsed laser deposition.It is higher that these preparation means are respectively provided with cost, and processing technology complexity etc. lacks
Point, it is restricted its application prospect.The hot pressing sintering method prepares coating mesh relatively low and relatively simple processing technology for cost
Preceding also no any report, and prepare the high-entropy alloy powder using mechanical alloying method and not yet have been reported that.Thus utilizing should
High-entropy alloy powder is a research emphasis by the simple process of the hot pressing sintering method prepares coating that how to succeed.
The content of the invention
It is an object of the present invention to for above shortcomings in the prior art, there is provided a kind of high-entropy alloy powder, this
Invention high-entropy alloy powder is prepared by mechanical alloying method, and final product is high-entropy alloy powder, the heat of alloy powder
Stability is good, and granule-morphology is more regular, is spherical or almost spherical, and particle size is more uniform.
Meanwhile present invention also offers above-mentioned high-entropy alloy powder is used, high-entropy alloy coating is prepared by hot pressed sintering
Method, the advantages that coating of formation is fine and close, without hole, flawless, and high with hardness, and sea water corrosion resistant is good.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of high-entropy alloy powder, counted according to atomic percentage conc sum for 100 %, its atomic percent is： Cu 18
The % of~23 %, Zr 18~23 %, Al 18~23 %, Ti 18~23 %, Ni 18~23.
Described high-entropy alloy powder, is made by mechanical alloying method, and ratio of grinding media to material used is 15~20 in mechanical milling process:1,
Ball milling revolution is 250~400 r/min, and Ball-milling Time is 100~120 h.
Described high-entropy alloy powder, granule-morphology are even-grained spherical or almost spherical.
Described high-entropy alloy powder, particle size range are 30~40 μm.
Described high-entropy alloy powder, preparing raw material are Cu, Zr, Al, Ti and Ni metal powder that purity is 99.9 more than %.
A kind of method that hot pressed sintering prepares high-entropy alloy coating：Matrix surface is pre-processed first, makes matrix table
Face cleaning is smooth, then inserts matrix in mould, then above-mentioned high-entropy alloy powder is preset on matrix, pre-set thickness 2
~5 mm, are then placed in hot-pressed sintering furnace, and coating is sintered on matrix under the protection of argon gas.
Described hot pressed sintering is multi-steps sintering：Stage one：200~350 DEG C, 5~15MPa, soaking time 10~
40min；Stage two：450~650 DEG C, 15~25MPa, 10~30min of soaking time；Stage three：800~1000 DEG C, 28~
50MPa, 25~60min of soaking time；Stage four：450~650 DEG C are cooled to, is depressurized to 0 MPa.
Described matrix is T8 steel；Described pretreatment, method are：Sand paper is polished, polishing, then with alcohol or acetone ultrasound
Ripple cleans, and finally with distilled water flushing and dries up.
The thickness of described coating is 0.6~1.2 mm.
Technical solution of the present invention advantage and principle are explained：(1) at present, it is gas atomization to prepare alloy powder common method
Method, powder size size prepared by gas atomization is extremely uneven, and particle surface is smooth to be spherical.Present invention selection uses machine
Tool alloying is directly successfully prepared high-entropy alloy powder, due to the continuous cold welding and agglomeration in mechanical milling process, final
Grain surface roughness is larger, but granule-morphology is more regular, and particle size is more uniform.Due to during hot pressed sintering, gas
The primary morphology and defect of powder prepared by atomization or mechanical alloying method can be genetic in sintered alloy, so of the invention
As a result show that the roughness on alloy powder particle surface prepared by mechanical alloying method is big and particle size is more uniform is advantageous to
Atoms permeating in the interface cohesion and sintering process of sintered powder.(2) laser cladding prepares coating is utilized in the prior art
Research it is more, laser melting and coating technique is to apply high energy in material surface, is allowed to that physicochemical change occurs, so as to change
The surface property of kind material.Because it is using high-energy-density, so cladding region between coating and matrix often be present,
The bad control in cladding region, and performance is unstable.For being a kind of brand-new idea using hot pressing and sintering technique prepares coating, heat
Pressure sintering pressurize from vertical direction while shaping powder in heating model, and is made the shaping of raw material powder and be sintered in together
A kind of moulding technique completed in one time the same space.The heating pressurization of hot pressed sintering is carried out simultaneously, and powder is always located
In hot plastic state, accelerate contact diffusion, the mass transfer flowing of particle, easily limit crystallite dimension and become big, be relatively easily available crystalline substance
Grain is tiny, product that consistency is high, and sinters cost and the energy is low, and processing technology is simple, there is indifferent gas in sintering process
The protection of body argon gas, protoxydic possibility drops.The present invention is successfully prepared with metal using this simple process
Gloss, compactness is good, without hole, the coating that hardness is high and resistance to corrosion seawater is good.
The advantage of the invention is that：High-entropy alloy powder is prepared using mechanical alloying method, and final product is high entropy
Alloy powder, the heat endurance of alloy powder is good, and granule-morphology is more regular, and particle size is more uniform.Using hot pressed sintering
Method prepares high-entropy alloy coating, and cost is low, and processing technology is simple, drops protoxydic possibility；The coating of sintering is fine and close, non-porous
Hole, flawless, the advantages that hardness is high and resistance to corrosion seawater is good, have a good application prospect.
Brief description of the drawings
Fig. 1 is the high-entropy alloy powder scanning electron microscope (SEM) photograph of embodiment 1；
Fig. 2 is the X ray diffracting spectrum of the high-entropy alloy coating of embodiment 4；
Fig. 3 is the scanning electron microscope (SEM) photograph and pictorial diagram of the high-entropy alloy coating of embodiment 4；
Fig. 4 is the hardness block diagram of the high-entropy alloy coating of embodiment 4 and matrix；
Fig. 5 is the electrochemical corrosion figure of the high-entropy alloy coating of embodiment 4 and matrix.
Embodiment
The present invention is further described with reference to specific embodiment, without departing from the idea case in the present invention described above,
The various replacements or change made according to ordinary skill knowledge and customary means, are included within the scope of the present invention.
Embodiment 1
A kind of high-entropy alloy powder, counted according to atomic percentage conc sum for 100 %, its atomic percent is： Cu
20%, Zr 21 %, Al 23%, Ti 18%, Ni 18%.
Mechanical alloying method prepares the present embodiment high-entropy alloy powder：According to said ratio, purity is selected to be all higher than 99.9
% simple metal element powders, add in ball mill, in 350 r/min, the h of ball milling 120, ratio of grinding media to material used is 15 in mechanical milling process
:1, obtain the high-entropy alloy powder that granularity is 35 μm.
The present embodiment high-entropy alloy powder granule-morphology is spherical or almost spherical, and the heat endurance of alloy powder is good.
Embodiment 2
A kind of high-entropy alloy powder, counted according to atomic percentage conc sum for 100 %, its atomic percent is： Cu
18%, Zr 18%, Al 18%, Ti 23%, Ni 23%.
Mechanical alloying method prepares the present embodiment high-entropy alloy powder：According to said ratio, purity is selected to be all higher than 99.9
% simple metal element powders, add in ball mill, in 250 r/min, the h of ball milling 100, ratio of grinding media to material used is 20 in mechanical milling process
:1, obtain the high-entropy alloy powder that granularity is 40 μm.
The present embodiment high-entropy alloy powder, granule-morphology is spherical or almost spherical, and the heat endurance of alloy powder is good.
Embodiment 3
A kind of high-entropy alloy powder, counted according to atomic percentage conc sum for 100 %, its atomic percent is： Cu
23%, Zr 23 %, Al 18%, Ti 18%, Ni 18%.
Mechanical alloying method prepares the present embodiment high-entropy alloy powder：According to said ratio, purity is selected to be all higher than 99.9
% simple metal element powders, add in ball mill, in 400 r/min, the h of ball milling 110, ratio of grinding media to material used is 18 in mechanical milling process
:1, obtain the high-entropy alloy powder that granularity is 38 μm.
The present embodiment high-entropy alloy powder granule-morphology is spherical or almost spherical, and the heat endurance of alloy powder is good.
Embodiment 4
A kind of method that hot pressed sintering prepares high-entropy alloy coating：T8 steel matrix surface is pre-processed first, method
For：Polished, and be processed by shot blasting using sand paper, carried out ultrasonic wave cleaning treatment using alcohol, finally entered with distilled water
Row is cleaned and dried up, and is made the cleaning of T8 steel surfaces smooth, is inserted in mould, the alloy powder of embodiment 1 is preset on T8 steel, in advance
It is 3mm to put thickness；It is then placed in hot-pressed sintering furnace, it is 0.9 ㎜ that coating is sintered in into thickness on matrix under the protection of argon gas.
Hot pressed sintering is multi-steps sintering：Stage one：300 DEG C, 10 MPa, it is incubated 15 min;Stage two：600 DEG C, 20 MPa, insulation 15
min；Stage three：950 DEG C, 30 MPa, it is incubated 30 min；Stage four：500 DEG C are cooled to, and is depressurized to 0 MPa.
Field emission microscopy observation is carried out to the high-entropy alloy powder of embodiment 1, as a result as shown in Figure 1.Can be with from Fig. 1
Find out that high-entropy alloy powder granule-morphology is spherical or almost spherical in embodiment 1, particle mean size is 35 μm.
X-ray diffraction analysis are carried out to the high-entropy alloy coating of embodiment 4, as a result as shown in Figure 2.As can be seen from Figure 2
The high-entropy alloy coating of embodiment 4 is shown as FCC, BCC and AlNi2Zr phases.
Field emission microscopy observation is carried out to the gained high-entropy alloy coating of embodiment 4, as a result as shown in Figure 3.From Fig. 3
As can be seen that the coating structure is fine and close, and tight, flawless.Its pictorial diagram display gained coating has obvious metallic luster, causes
Density etc. is consistent with scanning electron microscope (SEM) photograph.
Micro-hardness testing is carried out to the gained high-entropy alloy coating of embodiment 4, as shown in Figure 4.Fig. 4 shows that coating hardness can
Up to 964.06 ± 10 HV0.2, and matrix hardness is 230.9 ± 20 HV0.2, illustrate with FCC, BCC and AlNi2Zr phases are tied
The hardness of the dense coating of structure is apparently higher than matrix hardness.
Sea water corrosion resistant test is carried out to the gained high-entropy alloy coating of embodiment 4, as shown in Figure 5.It can be seen that in Fig. 5
The corrosion potential of shown coating is apparently higher than matrix, and coating has obvious passivation region, and secondary passivity area be present, says
The resistance to corrosion seawater of bright coating is substantially better than matrix.
Embodiment 5
A kind of method that hot pressed sintering prepares high-entropy alloy coating：T8 steel matrix surface is pre-processed first, method
For：Polished, and be processed by shot blasting using sand paper, carried out ultrasonic wave cleaning treatment using acetone, finally entered with distilled water
Row is cleaned and dried up, and is made the cleaning of T8 steel surfaces smooth, is inserted in mould, the alloy powder of embodiment 2 is preset on T8 steel, in advance
It is 2 mm to put thickness；It is then placed in hot-pressed sintering furnace, it is 0.7 that coating is sintered in into thickness on matrix under the protection of argon gas
㎜.Hot pressed sintering is multi-steps sintering：Stage one：200 DEG C, 5 MPa, it is incubated 10min;Stage two：450 DEG C, 15 MPa, insulation
10 min；Stage three：800 DEG C, 28 MPa, it is incubated 25 min；Stage four：450 DEG C are cooled to, and is depressurized to 0 MPa.
Micro-hardness testing is carried out to the gained high-entropy alloy coating of embodiment 5, the results showed that coating hardness is reachable
764.06 ± 15 HV0.2, and matrix hardness is 231.0 ± 18 HV0.2。
Embodiment 6
A kind of method that hot pressed sintering prepares high-entropy alloy coating：T8 steel matrix surface is pre-processed first, method
For：Polished, and be processed by shot blasting using sand paper, carried out ultrasonic wave cleaning treatment using acetone, finally entered with distilled water
Row is cleaned and dried up, and is made the cleaning of T8 steel surfaces smooth, is inserted in mould, the alloy powder of embodiment 3 is preset on T8 steel, in advance
It is 5 mm to put thickness；It is then placed in hot-pressed sintering furnace, it is 1.2 that coating is sintered in into thickness on matrix under the protection of argon gas
mm.Hot pressed sintering is multi-steps sintering：Stage one：350 DEG C, 15 MPa, it is incubated 40 min;Stage two：650 DEG C, 25 MPa, protect
30 min of temperature；Stage three：1000 DEG C, 50 MPa, it is incubated 60 min；Stage four：650 DEG C are cooled to, and is depressurized to 0MPa.
Micro-hardness testing is carried out to the gained high-entropy alloy coating of embodiment 6, the results showed that coating hardness is up to 854.12
± 15HV0.2, and matrix hardness is 228.9 ± 15HV0.2。
Claims (6)
1. a kind of method that hot pressed sintering prepares high-entropy alloy coating, it is characterised in that：Matrix surface is pre-processed first,
Make matrix surface cleaning smooth, then insert matrix in mould, then high-entropy alloy powder is preset on matrix, pre-set thickness
For 2~5 mm, it is then placed in hot-pressed sintering furnace, coating is sintered on matrix under the protection of argon gas；
The high-entropy alloy powder, counted according to atomic percentage conc sum for 100 %, its atomic percent is：Cu 18~23
The % of %, Zr 18~23 %, Al 18~23 %, Ti 18~23 %, Ni 18~23；
Described high-entropy alloy powder, particle size range are 30~40 μm, are made by mechanical alloying method, balls in mechanical milling process
Material is than being 15~20:1, ball milling revolution is 250~400 r/min, and Ball-milling Time is 100~120 h.
2. according to the method for claim 1, it is characterised in that：The high-entropy alloy powder, granule-morphology are epigranular
Spherical or almost spherical.
3. according to the method for claim 1, it is characterised in that：The high-entropy alloy powder, preparing raw material are that purity is
99.9 more than % Cu, Zr, Al, Ti and Ni metal powder.
4. according to the method for claim 1, it is characterised in that：Described hot pressed sintering is multi-steps sintering：Stage one：200
~350 DEG C, 5~15MPa, 10~40min of soaking time；Stage two：450~650 DEG C, 15~25MPa, soaking time 10~
30min；Stage three：800~1000 DEG C, 28~50MPa, 25~60min of soaking time；Stage four：It is cooled to 450~650
DEG C, it is depressurized to 0 MPa.
5. according to the method for claim 1, it is characterised in that：Described matrix is T8 steel；Described pretreatment, method are：
Sand paper is polished, polishing, is then cleaned with alcohol or acetone ultrasonic wave, finally with distilled water flushing and is dried up.
6. according to the method for claim 1, it is characterised in that：The thickness of described coating is 0.6~1.2 ㎜.
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| RU2808748C1 (en) * | 2022-12-28 | 2023-12-04 | федеральное государственное автономное образовательное учреждение высшего образования "Санкт-Петербургский политехнический университет Петра Великого" (ФГАОУ ВО "СПбПУ") | Method for producing spherical powder of high-entropy alloy boride |
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| CN107829007B (en) * | 2017-10-26 | 2019-11-19 | 福建工程学院 | A kind of method that high-entropy alloy and powder metallurgic method prepare high-entropy alloy block |
| CN110776311B (en) * | 2019-11-06 | 2021-07-30 | 常州大学 | Method for preparing perovskite type composite oxide high-entropy ceramic by hot-pressing sintering |
| CN111058076B (en) * | 2019-12-30 | 2020-11-20 | 安徽工业大学 | Zr-based high-entropy alloy material and method for synthesizing porous spherical structure on surface of Zr-based high-entropy alloy |
| CN113798495B (en) * | 2021-08-12 | 2023-07-18 | 西安理工大学 | High-entropy alloy sintering molding process with equivalent conversion of double elements |
| CN115094295B (en) * | 2022-06-23 | 2023-03-31 | 江苏科技大学 | High-entropy alloy powder, coating thereof and preparation method of coating |
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