CN106435407B - Preparation method of dumbbell-shaped iron-based block metal glass sample - Google Patents
Preparation method of dumbbell-shaped iron-based block metal glass sample Download PDFInfo
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- CN106435407B CN106435407B CN201610871540.6A CN201610871540A CN106435407B CN 106435407 B CN106435407 B CN 106435407B CN 201610871540 A CN201610871540 A CN 201610871540A CN 106435407 B CN106435407 B CN 106435407B
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- 239000002184 metal Substances 0.000 title claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 26
- 239000011521 glass Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title abstract description 37
- 229910052742 iron Inorganic materials 0.000 title abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000010453 quartz Substances 0.000 claims abstract description 49
- 239000005300 metallic glass Substances 0.000 claims abstract description 39
- 239000000956 alloy Substances 0.000 claims abstract description 33
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000010791 quenching Methods 0.000 claims abstract description 7
- 230000000171 quenching effect Effects 0.000 claims abstract description 7
- 239000003708 ampul Substances 0.000 claims description 46
- 238000000746 purification Methods 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 230000004224 protection Effects 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000011324 bead Substances 0.000 claims description 6
- 210000005239 tubule Anatomy 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 230000000994 depressogenic effect Effects 0.000 claims description 3
- 229910001338 liquidmetal Inorganic materials 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 238000005201 scrubbing Methods 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000012466 permeate Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 1
- 238000011160 research Methods 0.000 abstract description 12
- 238000012360 testing method Methods 0.000 abstract description 4
- 238000007664 blowing Methods 0.000 abstract 1
- 238000009864 tensile test Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 36
- 238000002474 experimental method Methods 0.000 description 11
- 230000006835 compression Effects 0.000 description 8
- 238000007906 compression Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000003814 drug Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000010953 base metal Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 229910000976 Electrical steel Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 210000003027 ear inner Anatomy 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 210000003128 head Anatomy 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012521 purified sample Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/22—Moulds for peculiarly-shaped castings
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/003—Making ferrous alloys making amorphous alloys
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a preparation method of a dumbbell-shaped iron-based block metallic glass sample, which comprises the steps of firstly preparing a master alloy ingot, then purifying the prepared master alloy ingot, blowing the dumbbell-shaped master alloy ingot out of a quartz tube to prepare a dumbbell-shaped quartz tube, finally placing the purified master alloy ingot into the dumbbell-shaped quartz tube, and then preparing the dumbbell-shaped metallic glass sample by water quenching internal melt. The method of the invention is the only method which can prepare the iron-based metal glass dumbbell-shaped test sample at present. The dumbbell-shaped metal glass sample can be used for tensile test after being prepared, so that the research range of the mechanical property of the iron-based metal glass can be widened, and the mechanical property of the iron-based metal glass can be more intrinsically represented. The research gap in the direction can be filled up by using the method for preparing the dumbbell-shaped iron-based metal glass sample, and a breakthrough result is expected to be obtained.
Description
Technical field
The invention belongs to glassy metal technical field, more particularly to the Fe-based bulk metallic glass of a kind of completely amorphous state of structure
The preparation method of glass dumbbell shaped tensile sample.
Background technology
Glassy metal is a kind of new amorphous state alloy material, and atomic arrangement does not have three-dimensional periodic, but several
Certain order is still showed within the scope of atomic distance, there are the performances such as excellent physics, chemistry, mechanics, is expected to become branch
The critical material of the new and high technologies such as the following precision machinery of support, information, aerospace, national defense industry.Iron based metallic glass is constituent element
The maximum a kind of glassy metal system of middle atomic percent iron, saturation magnetization can be less than in 1.0~1.7T, coercivity
Up to 450000, soft magnet performance is much better than traditional silicon steel sheet for 1.0A/m, magnetic conductivity, can directly cast molten processing or 3D printing at
The magnetic core and device of various labyrinths are the ideal magnetic functions such as energy-economic transformer, inductor, radio-frequency identification tag
Material.In addition, its corrosion resistance is 10000 times higher than conventional stainless steel, fracture strength is great up to 4GPa or more, and one kind
The structural material of application potential.It is studied according to american society for metals, if steel strength can improve 5%, bridge life will increase
1%, economic benefit is up to 30,000,000,000 dollars；Based bulk metallic glasses fracture strength is high, up to several times to more than ten times of carbon steel,
If it can be applied to structural material, the economic benefit of generation is even more to be difficult to estimate.In recent years, in the unremitting effort of researcher
Under, the compression plasticity of based bulk metallic glasses is constantly promoted.However, compression experiment belong to restricted type experiment, sample end face with
Frictional force between pressure head can influence the compression deformation and failure mode of sample, seriously affect the deformation row of iron based metallic glass
To promote a large amount of shear bands to generate, to bear the strain energy applied, leading to the intrinsic power of compression performance non-ferric base metal glass
Characteristic is learned, based bulk metallic glasses plastic flow mechanism research is hindered.And stretching experiment belongs to expanding experiment, experiment instrument
Device substantially will not have an impact the compression deformation and failure mode of experiment material, so can more reflect the intrinsic category of material
Property.Therefore, it is the field " Holy grail " that seeking, which has the metal glass material of stretching plastic, and research based bulk metallic glasses exist
Fracture damage mechanism is more favorable to go deep into understanding and disclose the deformation failure essence of glassy metal in tensile stress field, has important
Scientific meaning.However, the critical dimension very little of presently found super large compression plasticity based bulk metallic glasses, less than
2.5mm, routine experiment method does not prepare " dumbbell shaped " tensile sample of the completely amorphous state of structure so far, currently, existing grind
It can only be the directly identical cylindrical metal glass bar in both ends to study carefully prepare.The present invention's is a kind of glassy metal examination of dumbbell shaped
Sample, both ends are thick intermediate thin, and whether suction casting method or spray to cast method are not all prepared not come out this sample before making the present invention, reason iron
The amorphous formation ability of base metal glass is small, and the demand that conventional method prepares dumbbell shaped sample is not achieved.
Invention content
It is existing to solve the object of the present invention is to provide a kind of preparation method of dumbbell shaped based bulk metallic glasses sample
The problem of dumbbell shaped tensile sample of the completely amorphous state of structure can not be prepared in technology.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of preparation method of dumbbell shaped based bulk metallic glasses sample, it is characterised in that：Include the following steps：
Step 1, the preparation of master alloy ingot：The chemical formula of the master alloy ingot is Fe80-x(Ni, Cr, Mo)x(P,B)y(C,
Si)z, wherein y+z=20；The raw material for preparing above-mentioned master alloy ingot is：Fe particles, Ni particles, Fe3P powder, Cr powder, Mo powder, B
Particle, Si powder and graphite powder；According to the ingredient of master alloy ingot, each raw material is weighed, then each raw material is put into washed in advance and is done
In dry quartz glass tube, quartz glass tube is accessed in vacuum extractor and is vacuumized；High-purity Ar is filled with into quartz glass tube
Gas vacuumizes again, carries out gas washing；Finally, the Ar gas that 0.85atm is passed through into quartz glass tube does protective gas, utilizes
1400~2000 DEG C of firelock heated quartz glass bottom of the tube, permeate a liquid metal bead after each element heating fusing；
After whole elements incorporate bead, by quartz glass tube quenching in cold water, master alloy ingot is obtained；
Step 2, the purification of master alloy ingot：By B2O3With CaO according to 3：1 mass ratio mixing will be mixed as purification medium
The purification medium got togather, which is placed in the quartz ampoule sealed to vacuumize to be placed on after ten minutes in 1250 DEG C of high temperature furnace, to be heated,
Medium to be purified be completely melt it is transparent install, open quartz ampoule, by step 1 synthesize master alloy ingot be put into purification medium in,
4 hours or more are kept the temperature at 1250 DEG C；
Step 3, the preparation of dumbbell shaped quartz ampoule：After quartz ampoule is heated to molten condition by firelock, in quartz ampoule two
Uniform load is held, quartz ampoule elongation is referred into required length, keeps quartz ampoule both ends relative position to fix, leaves firelock high-temperature region,
Make quartz ampoule natural cooling, that is, prepares dumbbell shaped quartz ampoule；
Step 4, the preparation of dumbbell shaped metal glass sample：One end closure of dumbbell shaped quartz ampoule prepared by step 3
Afterwards, vacuum extractor is accessed after the master alloy ingot after step 2 purifies being placed on quartz ampoule, using identical with step 1
Method vacuumize and after gas washing, under the protection of the Ar gas of 0.85atm, with firelock heating alloy to melting, then takes out true
Empty 10s removals protection gas, then molten metal ball is got lodged in into tubule port, it is filled with Ar gas, is depressed into molten metal using air pressure
After in dumbbell shaped tubule, quartz ampoule is placed in 1250 DEG C of high temperature furnace keeps the temperature immediately, taken out and be immediately placed in cold water after 1 minute
Quenching, to obtain dumbbell shaped based bulk metallic glasses sample.
In the step 1, the vacuum degree in quartz glass tube is 30Pa or less.
In the step 1, gas scrubbing carries out 4-5 times.
In step 2, during master alloy ingot is put into purification medium heat-preserving, stone is taken out from high temperature furnace at interval of half an hour
Ying Guan sees that sample crosses cool time from be fetched into recalescence, when cool time reach maximum value and when keeping stablizing, into quartz ampoule
It is filled with the Ar gas for being slightly less than an atmospheric pressure, quartz ampoule is quenched, takes out sample, is dried with after alcohol washes, for future use.
In step 3, the original size of the quartz ampoule is：1 centimetre of diameter, 1 millimeter of wall thickness.
The beneficial effects of the invention are as follows：
The it is proposed of the invention blows out dumbbell shaped first with quartz ampoule, and then water quenching inner melt prepares dumbbell shaped
Metal glass sample, method of the invention are the currently the only methods that can prepare based bulk metallic glasses dumbbell-shaped specimen.
The non-crystal bar of column prepares can only do compression experiment, therefore, based bulk metallic glasses mechanical property at present
Research mainly research Compressive Mechanical Properties；But the metal glass sample of dumbbell shaped can do stretching in fact after preparing
It tests, this can widen the research range of based bulk metallic glasses mechanical property, more intrinsic characterization iron based metallic glass
Mechanical property.The research in this direction can be filled up by preparing dumbbell shaped based bulk metallic glasses sample using the method for the present invention
Blank is expected to the achievement of making a breakthrough property.
Description of the drawings
Fig. 1 is the dumbbell shaped quartz ampoule prepared in the present invention；
Fig. 2 is dumbbell shaped based bulk metallic glasses sample prepared by the present invention；
Fig. 3 is that the XRD and DSC of different shape based bulk metallic glasses scheme.
Specific implementation mode
The present invention is further described with reference to specific embodiment.
Embodiment
The preparation method of the dumbbell shaped based bulk metallic glasses sample of the present embodiment, includes the following steps：
(1) preparation of master alloy ingot：The chemical formula of master alloy ingot is Fe80-x(Ni, Cr, Mo)x(P,B)y(C,Si)z,
In, y+z=20；The raw material for preparing above-mentioned master alloy ingot is：Fe particles (purity 99.98%), Ni particles (purity 99.7%),
Fe3P powder (purity 99.9%), Cr powder (purity 99.9%), Mo powder (purity 99.9%), B particles (purity 99.9%), Si powder
(purity 99.99%) and graphite powder (purity 99.9995%).According to the alloying component set in proportion in precision as 10-5The electricity of g
Claim on sub- balance after drug, drug is put into the quartz glass tube of drying washed in advance, quartz glass tube is accessed real
It is vacuumized in experiment device, the vacuum degree in quartz glass tube is in 30Pa or less.High-purity Ar gas is filled with into quartz glass tube, again
It vacuumizes, such gas scrubbing carries out 4-5 times.Finally, the Ar gas that 0.85atm or so is passed through into quartz ampoule does protection gas
Body is permeated a using the drug of 1400~2000 DEG C of firelock heated quartz glass bottom of the tube after each element heating fusing
Liquid metal bead.After whole elements incorporate bead, by quartz glass tube quenching in cold water, master alloy ingot is obtained.
(2) purification of master alloy ingot：By B2O3It is mixed according to following mass ratio with CaO：B2O3：CaO=3：1, it will mix
Good purification medium, which is placed in the quartz ampoule sealed to vacuumize to be placed on after ten minutes in 1250 DEG C of high temperature furnace, to be heated, and is waited for
Purification medium be completely melt it is transparent install, open quartz ampoule, by the master alloy ingot synthesized before be put into purification medium in,
Keep the temperature 4 hours under at 1250 DEG C or more.During this, quartz ampoule can be taken out from high temperature furnace at interval of half an hour, see sample certainly
Be fetched into recalescence crosses cool time, when cool time reach maximum value and when keeping stablizing, be filled with into quartz ampoule and be slightly less than one
The Ar gas of a atmospheric pressure, quartz ampoule is quenched, and takes out sample, is dried with after alcohol washes, for future use.
(3) preparation of dumbbell shaped quartz ampoule：By about 1 centimetre of diameter, the quartz ampoule that 1 millimeter or so of wall thickness passes through Bench
After burners114/1PSL an firelocks are heated to molten condition, in quartz ampoule both ends uniform load, quartz ampoule elongation is referred into institute
Length is needed, keeps quartz ampoule both ends relative position to fix, leaves firelock high-temperature region, make quartz ampoule natural cooling, that is, prepare mute
Bell-shaped quartz ampoule, as shown in Figure 1.
(4) preparation of dumbbell shaped metal glass sample：After an end closure of dumbbell shaped quartz ampoule, after oxide is purified
Sample be placed on quartz ampoule special in this way after access experimental system, vacuumized using the identical method with step (1)
And after gas washing, under the protection of the Ar gas of 0.85atm, with firelock heating alloy to melting, 10s removal protections are then vacuumized
Gas, then molten metal ball is got lodged in into tubule port, it is filled with Ar gas, molten metal is depressed into dumbbell shaped tubule using air pressure
Afterwards, quartz ampoule is placed in 1250 DEG C of high temperature furnace immediately and is kept the temperature, taken out after about 1 minute and be immediately placed in cold quenching-in water, to
Dumbbell shaped based bulk metallic glasses sample is obtained, as shown in Figure 2.
The structure detection of dumbbell shaped metal glass sample：
X-ray diffractometer (XRD) detects：A part is taken to get off the dumbbell shaped metal glass sample prepared, then totally
Container in smash, grind into powder, precipitated phase is detected on X-ray diffractometer.
Differential scanning calorimeter (DSC) detects：Sample quality is weighed with the precision electronic balance that precision is 0.1mg.It will be golden
Belong to glass sample and the temperature near the exothermic peak of supercooling liquid phase region is heated to the heating rate of 0.67K/s by DSC, then cools down
To room temperature, the sample after being heat-treated these carries out dsc analysis, observes the variation of exothermic peak.
XRD and DSC experiments show that the above-mentioned ferrous alloy stick prepared and dumbbell shaped alloy are non crystalline structure, such as Fig. 3
Shown, as qualified dumbbell shaped metal glass sample.If DSC does not have apparent exothermic peak or XRD to have apparent crystallization
Peak, from the beginning survey repeats the above steps, until obtaining testing result sample as shown in Figure 3.
Study that prepare can only be the directly identical cylindrical metal glass bar in both ends currently, existing, and the present invention's is
A kind of based bulk metallic glasses sample of dumbbell shaped, both ends are thick intermediate thin, and this sample is whether inhaled before making the present invention
Casting or spray to cast method are not all prepared not come out, and the amorphous formation ability of reason iron based metallic glass is small, and conventional method system is not achieved
The demand of standby dumbbell shaped sample.
The it is proposed of the invention blows out dumbbell shaped first with quartz ampoule, and then water quenching inner melt prepares dumbbell shaped
Metal glass sample, this method are the currently the only methods that can prepare based bulk metallic glasses dumbbell-shaped specimen.
The non-crystal bar of column prepares can only do compression experiment, therefore, based bulk metallic glasses mechanical property at present
Research mainly research Compressive Mechanical Properties；But the metal glass sample of dumbbell shaped can do stretching in fact after preparing
It tests, this can widen the research range of iron based metallic glass mechanical property, the mechanics of more intrinsic characterization iron based metallic glass
Performance.This method has also obtained the affirmative and favorable comment of multidigit expert in field, it is believed for preparing dumbbell shaped iron-based gold using this method
Belong to the research blank that glass specimen can fill up this direction, is expected to the achievement of making a breakthrough property.
The above is only a preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (4)
1. a kind of preparation method of dumbbell shaped based bulk metallic glasses sample, it is characterised in that：Include the following steps：
Step 1, the preparation of master alloy ingot：The chemical formula of the master alloy ingot is Fe80-x(Ni, Cr, Mo)x(P, B)y(C,
Si)z , wherein y+z=20；The raw material for preparing above-mentioned master alloy ingot is：Fe particles, Ni particles, Fe3P powder, Cr powder, Mo powder, B
Particle, Si powder and graphite powder；According to the ingredient of master alloy ingot, each raw material is weighed, then each raw material is put into washed in advance and is done
In dry quartz glass tube, quartz glass tube is accessed in vacuum extractor and is vacuumized；High-purity Ar is filled with into quartz glass tube
Gas vacuumizes again, carries out gas washing；Finally, the Ar gas that 0.85atm is passed through into quartz glass tube does protective gas, utilizes
1400 ~ 2000 DEG C of firelock heated quartz glass bottom of the tube, permeate a liquid metal bead after each element heating fusing；It waits for
After whole elements incorporate bead, by quartz glass tube quenching in cold water, master alloy ingot is obtained；
Step 2, the purification of master alloy ingot：By B2O3With CaO according to 3：1 mass ratio mixing will be mixed as purification medium
Purification medium be placed in the quartz ampoule sealed to vacuumize to be placed on after ten minutes in 1250 DEG C of high temperature furnace and heat, wait carrying
Prefect dielectric be completely melt it is transparent, open quartz ampoule, by step 1 synthesize master alloy ingot be put into purification medium in, at 1250 DEG C
Lower heat preservation 4 hours or more；
Step 3, the preparation of dumbbell shaped quartz ampoule：It is equal at quartz ampoule both ends after quartz ampoule is heated to molten condition by firelock
Quartz ampoule is elongated to required length by even load, is kept quartz ampoule both ends relative position to fix, is left firelock high-temperature region, make stone
English pipe natural cooling, that is, prepare dumbbell shaped quartz ampoule；
Step 4, the preparation of dumbbell shaped metal glass sample：It, will after one end closure of dumbbell shaped quartz ampoule prepared by step 3
Master alloy ingot after step 2 purifies accesses vacuum extractor after being placed on quartz ampoule, using method identical with step 1 into
Row vacuumizes and after gas washing, under the protection of the Ar gas of 0.85atm, with firelock heating alloy to melting, then vacuumizes 10s and goes
Except protection gas, then molten metal ball got lodged in into tubule port, be filled with Ar gas, it is thin that molten metal is depressed into dumbbell shaped using air pressure
Quartz ampoule is placed in 1250 DEG C of high temperature furnace keeps the temperature immediately by Guan Zhonghou, is taken out after 1 minute and is immediately placed in cold quenching-in water, from
And obtain dumbbell shaped based bulk metallic glasses sample.
2. the preparation method of dumbbell shaped based bulk metallic glasses sample according to claim 1, it is characterised in that：It is described
In step 1, the vacuum degree in quartz glass tube is 30Pa or less.
3. the preparation method of dumbbell shaped based bulk metallic glasses sample according to claim 1, it is characterised in that：It is described
In step 1, gas scrubbing carries out 4-5 times.
4. the preparation method of dumbbell shaped based bulk metallic glasses sample according to claim 1, it is characterised in that：Step
In three, the original size of the quartz ampoule is：1 centimetre of diameter, 1 millimeter of wall thickness.
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