CN106435407A - Preparation method of dumbbell-shaped iron base block metal glass sample - Google Patents
Preparation method of dumbbell-shaped iron base block metal glass sample Download PDFInfo
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- CN106435407A CN106435407A CN201610871540.6A CN201610871540A CN106435407A CN 106435407 A CN106435407 A CN 106435407A CN 201610871540 A CN201610871540 A CN 201610871540A CN 106435407 A CN106435407 A CN 106435407A
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- quartz ampoule
- dumbbell
- dumbbell shaped
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- 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
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- 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
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- 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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Abstract
The invention discloses a preparation method of a dumbbell-shaped iron base block metal glass sample. Firstly, a master alloy ingot is prepared; then, the prepared master alloy ingot is purified; a quartz pipe is used for blowing out a dumbbell shape to prepare a dumbbell-shaped quartz pipe; finally, the purified master alloy ingot is put in the dumbbell-shaped quartz pipe; and then, an internal melt is quenched by water to prepare the dumbbell-shaped metal glass sample. The method is unique method capable of preparing the iron base metal glass dumbbell-shaped sample at present. The prepared dumbbell-shaped metal glass sample can perform a stretching test to widen the research range of the iron base metal glass mechanical performance to represent the iron base metal glass mechanical performance more intrinstically. The method for preparing the dumbbell-shaped iron base metal glass sample can fill blank of the research blank in the direction, and is hopeful to achieve breakthrough results.
Description
Technical field
The invention belongs to metal glass technical field, particularly to a kind of Fe-based bulk metallic glass of the completely amorphous state of structure
The preparation method of glass dumbbell shaped tensile sample.
Background technology
Metal glass is a kind of new amorphous state alloy material, and its atomic arrangement does not have three-dimensional periodic, but several
Still present certain order in the range of atomic distance, there is the performances such as excellent physics, chemistry, mechanics, be expected to become and prop up
The critical material of the new and high technologies such as the following precision optical machinery of support, information, Aero-Space, national defense industry.Iron based metallic glass is constituent element
The maximum metalloid glass 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 stalloy for 1.0A/m, pcrmeability, can directly cast molten processing or 3D printing becomes
The magnetic core of various labyrinths and device, are the preferably magnetic functions such as energy-economic transformer, inducer, radio-frequency identification tag
Material.Additionally, its decay resistance is higher than conventional rustless steel 10000 times, fracture strength, up to more than 4GPa, is also that a class is great
The structural material of application potential.According to american society for metals's research, if steel strength can improve 5%, bridge life will increase
1%, economic benefit reaches 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 difficult to estimate.In recent years, in the unremitting effort of research worker
Under, the compression plasticity of based bulk metallic glasses is constantly lifted.However, compression experiment belong to restricted type test, sample end face with
Frictional force between pressure head can affect compress variation and the failure mode of sample, has a strong impact on the deformation row of iron based metallic glass
For promoting a large amount of shear bands to generate, thus bearing the strain energy of applying, leading to the intrinsic power of compression performance non-ferric base metal glass
Learn characteristic, hinder based bulk metallic glasses plastic flow mechanism research.And stretching experiment belongs to expanding test, experiment instrument
Device will not produce impact to the compress variation of experiment material and failure mode substantially, so the intrinsic genus of material more can be reflected
Property.Therefore, the metal glass material seeking to have stretching plastic is this field " Holy grail ", and research based bulk metallic glasses exist
In tension field, fracture damage mechanism is more favorable to the deep deformation failure essence understanding and disclosing metal glass, has important
Scientific meaning.However, the critical dimension very little of the super large compression plasticity based bulk metallic glasses having now been found that, less than
2.5mm, normal experiment method does not prepare " dumbbell shaped " tensile sample of the completely amorphous state of structure so far, at present, existing grinds
Study carefully that prepare can only be two ends direct identical cylindrical metal Glass rod.The present invention be a kind of dumbbell shaped metal glass examination
Sample, two ends slightly in the middle of thin, this sample before making the present invention whether suction casting method or spray to cast method all can not prepare out, reason ferrum
The amorphous formation ability of base metal glass is little, does not reach the demand that traditional method prepares dumbbell shaped sample.
Content of the invention
It is an object of the invention to provide a kind of preparation method of dumbbell shaped based bulk metallic glasses sample, existing to solve
The problem of the dumbbell shaped tensile sample of the completely amorphous state of structure cannot be prepared in technology.
For achieving the above object, the technical solution used in the present invention is：
A kind of preparation method of dumbbell shaped based bulk metallic glasses sample it is characterised in that：Comprise the following steps：
Step one, the preparation of master alloy ingot：The chemical formula of described master alloy ingot is Fe80-x(Co, Ni, Cr, Mo)x(P,B)y
(C,Si)z, wherein, y+z=20；The raw material preparing above-mentioned master alloy ingot is：Fe granule, Ni granule, Fe3P powder, Cr powder, Mo
Powder, B granule, Si powder and graphite powder；According to the composition of master alloy ingot, weigh each raw material, then each raw material is put into and wash in advance
And in the quartz glass tube being dried, quartz glass tube is accessed evacuation in vacuum extractor；It is filled with height into quartz glass tube
Pure Ar gas, evacuation again, carry out gas washing；Finally, the Ar gas being passed through 0.85atm toward in quartz glass tube does protective gas, profit
With 1400～2000 DEG C of firelock heated quartz glass bottom of the tube, a liquid metal that permeates after each element heating fusing is little
Ball；After whole elements incorporate bead, quartz glass tube is quenched in cold water, obtains master alloy ingot；
Step 2, the purification of master alloy ingot：By B2O3With CaO according to 3：1 mass ratio mixing, as purification medium, will mix
The purification medium getting togather is placed on evacuation in the quartz ampoule sealed and, after 10 minutes, is placed on heating in 1250 DEG C of high temperature furnace,
Medium to be purified be completely melt transparent install, open quartz ampoule, the master alloy ingot that step one is synthesized put into purification medium in,
It is incubated more than 4 hours at 1250 DEG C；
Step 3, the preparation of dumbbell shaped quartz ampoule：Quartz ampoule is heated to after molten condition by firelock, in quartz ampoule two
End uniform load, quartz ampoule is elongated and refers to Len req, keeps quartz ampoule two ends relative position to fix, leaves firelock high-temperature region,
Make quartz ampoule natural cooling, that is, prepare 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, the master alloy ingot after purifying through step 2 is placed on access vacuum extractor after quartz ampoule, adopts and step one identical
After method carries out evacuation gas washing, under the protection of the Ar gas of 0.85atm, with firelock heating alloy to melting, then take out true
Empty 10s removes shielding gas, then the metal ball of melting is got lodged in tubule port, is filled with Ar gas, is depressed into motlten metal using air pressure
After in dumbbell shaped tubule, immediately quartz ampoule is placed on insulation in 1250 DEG C of high temperature furnace, takes out after 1 minute and be immediately placed in cold water
Quenching, thus obtain dumbbell shaped based bulk metallic glasses sample.
In described step one, the vacuum in quartz glass tube is below 30Pa.
In described step one, gas scrubbing is carried out 4-5 time.
In step 2, during master alloy ingot puts into purification medium heat-preserving, take out stone at interval of half an hour from high temperature furnace
Ying Guan, see sample from be fetched into recalescence cross cool time, whne cool time reach maximum and keep stable when, in quartz ampoule
It is filled with the Ar gas being slightly less than an atmospheric pressure, quartz ampoule is quenched, take out sample, with being dried after alcohol washes, for future use.
In step 3, the original size of described quartz ampoule is：1 centimetre of diameter, 1 millimeter of wall thickness.
The invention has the beneficial effects as follows：
The proposition of the invention blows out dumbbell shaped first with quartz ampoule, and then water quenching inner melt prepares dumbbell shaped
Metal glass sample, the method for the present invention is the currently the only method that can prepare based bulk metallic glasses dumbbell-shaped specimen.
The non-crystal bar of column prepares and can only do compression experiment, therefore, current based bulk metallic glasses mechanical property
Research is mainly studies Compressive Mechanical Properties；But the metal glass sample of dumbbell shaped can do stretching after preparing real
Test, this can widen the research range of based bulk metallic glasses mechanical property, more intrinsic sign iron based metallic glass
Mechanical property.Prepare the research that dumbbell shaped based bulk metallic glasses sample can fill up this direction using the method for the present invention
Blank, is expected to the achievement of making a breakthrough property.
Brief description
Fig. 1 is the dumbbell shaped quartz ampoule of preparation in the present invention；
The dumbbell shaped based bulk metallic glasses sample that Fig. 2 is prepared for the present invention；
Fig. 3 is the XRD and DSC figure of different shape based bulk metallic glasses.
Specific embodiment
With reference to specific embodiment, the present invention is further described.
Embodiment
The preparation method of the dumbbell shaped based bulk metallic glasses sample of the present embodiment, comprises the following steps：
(1) preparation of master alloy ingot：The chemical formula of master alloy ingot is Fe80-x(Co, Ni, Cr, Mo)x(P,B)y(C,Si)z,
Wherein, y+z=20；The raw material preparing above-mentioned master alloy ingot is：Fe granule (purity 99.98%), Ni granule (purity 99.7%),
Fe3P powder (purity 99.9%), Cr powder (purity 99.9%), Mo powder (purity 99.9%), B granule (purity 99.9%), Si powder
(purity 99.99%) and graphite powder (purity 99.9995%).According to the alloying component setting in proportion in precision as 10-5The electricity of g
Claim on sub- balance after medicine, medicine is put in the quartz glass tube of the drying washed in advance, quartz glass tube is accessed real
Evacuation in experiment device, the vacuum in quartz glass tube is in below 30Pa.It is filled with high-purity Ar gas into quartz glass tube, again
Evacuation, such gas scrubbing is carried out 4-5 time.Finally, be passed through toward in quartz ampoule 0.85atm about Ar gas do shielding gas
Body, using the medicine of 1400～2000 DEG C of firelock heated quartz glass bottom of the tube, permeates after each element heating fusing individual
Liquid metal bead.After whole elements incorporate bead, quartz glass tube is quenched in cold water, obtains master alloy ingot.
(2) purification of master alloy ingot：By B2O3Mix according to following mass ratio with CaO：B2O3：CaO=3：1, will mix
Good purification medium is placed on evacuation in the quartz ampoule sealed and, after 10 minutes, is placed on heating in 1250 DEG C of high temperature furnace, treats
Purification medium be completely melt transparent install, open quartz ampoule, by the master alloy ingot synthesizing before put into purification medium in,
Lower insulation more than 4 hours at 1250 DEG C.During this, quartz ampoule can be taken out at interval of half an hour from high temperature furnace, see sample certainly
Be fetched into recalescence cross cool time, whne cool time reach maximum and keep stable when, be filled with quartz ampoule and be slightly less than one
The Ar gas of individual atmospheric pressure, quartz ampoule is quenched, and takes out sample, with being dried after alcohol washes, for future use.
(3) preparation of dumbbell shaped quartz ampoule：By about 1 centimetre of diameter, the quartz ampoule of wall thickness 1 millimeter passes through Bench
After burners114/1PSL an firelock is heated to molten condition, in quartz ampoule two ends uniform load, quartz ampoule is elongated and refers to institute
Need length, keep quartz ampoule two ends relative position to fix, leave 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 after so special quartz ampoule and access experimental system, using carrying out evacuation with step (1) identical method
And after gas washing, under the protection of the Ar gas of 0.85atm, with firelock heating alloy to melting, then evacuation 10s removes protection
Gas, then the metal ball of melting is got lodged in tubule port, it is filled with Ar gas, using air pressure, motlten metal is depressed in dumbbell shaped tubule
Afterwards, immediately quartz ampoule is placed on insulation in 1250 DEG C of high temperature furnace, takes out after about 1 minute and be immediately placed in cold quenching-in water, thus
Obtain dumbbell shaped based bulk metallic glasses sample, as shown in Figure 2.
The structure detection of dumbbell shaped metal glass sample：
X-ray diffractometer (XRD) detects：The dumbbell shaped prepared metal glass sample is taken a part to get off, more totally
Container in smash, grind into powder, on X-ray diffractometer detect precipitated phase.
Differential scanning calorimeter (DSC) detects：Sample quality precision is that the precision electronic balance of 0.1mg weighs.By gold
Belong to the temperature that glass sample is heated near the exothermic peak of supercooling liquid phase region by DSC with the heating rate of 0.67K/s, then cool down
To room temperature, the sample after these heat treatments is being carried out dsc analysis, is observing the change of exothermic peak.
XRD and DSC experiment shows, the above-mentioned ferrous alloy rod 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 obvious exothermic peak or XRD to have obvious crystallization
Peak, surveys from the beginning repeat the above steps, till obtaining testing result sample as shown in Figure 3.
At present, what existing research was prepared can only be two ends direct identical cylindrical metal Glass rod, and the present invention's is
A kind of based bulk metallic glasses sample of dumbbell shaped, its two ends is slightly middle thin, and this sample is whether inhaled before making the present invention
Casting or spray to cast method all can not be prepared out, and the amorphous formation ability of reason iron based metallic glass is little, does not reach traditional method system
The demand of standby dumbbell shaped sample.
The proposition of the invention blows out dumbbell shaped first with quartz ampoule, and then water quenching inner melt prepares dumbbell shaped
Metal glass sample, the method is the currently the only method that can prepare based bulk metallic glasses dumbbell-shaped specimen.
The non-crystal bar of column prepares and can only do compression experiment, therefore, current based bulk metallic glasses mechanical property
Research is mainly studies Compressive Mechanical Properties；But the metal glass sample of dumbbell shaped can do stretching after preparing real
Test, this can widen the research range of iron based metallic glass mechanical property, the mechanics of more intrinsic sign iron based metallic glass
Performance.The method has also obtained the affirmative of multidigit expert and favorable comment in field it is believed that preparing dumbbell shaped iron-based gold using the method
Belong to the research blank that glass specimen can fill up this direction, be expected to the achievement of making a breakthrough property.
The above be only the preferred embodiment of the present invention it should be pointed out that：Ordinary skill people for the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of dumbbell shaped based bulk metallic glasses sample it is characterised in that：Comprise the following steps：
Step one, the preparation of master alloy ingot：The chemical formula of described master alloy ingot is Fe80-x(Co, Ni, Cr, Mo)x(P,B)y(C,
Si)z, wherein, y+z=20；The raw material preparing above-mentioned master alloy ingot is：Fe granule, Ni granule, Fe3P powder, Cr powder, Mo powder, B
Granule, Si powder and graphite powder；According to the composition of master alloy ingot, weigh each raw material, then each raw material is put into and wash in advance and do
In dry quartz glass tube, quartz glass tube is accessed evacuation in vacuum extractor；It is filled with high-purity Ar into quartz glass tube
Gas, evacuation again, carry out gas washing；Finally, the Ar gas being passed through 0.85atm toward in quartz glass tube does protective gas, utilizes
1400～2000 DEG C of firelock heated quartz glass bottom of the tube, permeate after each element heating fusing a liquid metal bead；
After whole elements incorporate bead, quartz glass tube is quenched in cold water, obtains master alloy ingot；
Step 2, the purification of master alloy ingot：By B2O3With CaO according to 3：1 mass ratio mixing, as purification medium, will mix
Purification medium be placed in the quartz ampoule sealed evacuation after 10 minutes, be placed on heating in 1250 DEG C of high temperature furnace, wait to carry
Prefect dielectric be completely melt transparent install, open quartz ampoule, the master alloy ingot that step one is synthesized put into purification medium in,
It is incubated more than 4 hours at 1250 DEG C；
Step 3, the preparation of dumbbell shaped quartz ampoule：Quartz ampoule is heated to after molten condition by firelock, equal at quartz ampoule two ends
Even loading, quartz ampoule is elongated and refers to Len req, keeps quartz ampoule two ends relative position to fix, leaves 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：After one end closure of dumbbell shaped quartz ampoule prepared by step 3, will
Master alloy ingot after step 2 purification is placed on access vacuum extractor after quartz ampoule, enters using with step one identical method
After row evacuation gas washing, under the protection of the Ar gas of 0.85atm, with firelock heating alloy to melting, then evacuation 10s goes
Except shielding gas, then the metal ball of melting is got lodged in tubule port, be filled with Ar gas, using air pressure, motlten metal is depressed into dumbbell shaped thin
Quartz ampoule is placed on insulation in 1250 DEG C of high temperature furnace, takes out and be immediately placed in cold quenching-in water after 1 minute by Guan Zhonghou immediately, from
And obtain dumbbell shaped based bulk metallic glasses sample.
2. dumbbell shaped based bulk metallic glasses sample according to claim 1 preparation method it is characterised in that：Described
In step one, the vacuum in quartz glass tube is below 30Pa.
3. dumbbell shaped based bulk metallic glasses sample according to claim 1 preparation method it is characterised in that：Described
In step one, gas scrubbing is carried out 4-5 time.
4. dumbbell shaped based bulk metallic glasses sample according to claim 1 preparation method it is characterised in that：Step
In two, during master alloy ingot puts into purification medium heat-preserving, take out quartz ampoule at interval of half an hour from high temperature furnace, see sample certainly
Be fetched into recalescence cross cool time, whne cool time reach maximum and keep stable when, be filled with quartz ampoule and be slightly less than one
The Ar gas of individual atmospheric pressure, quartz ampoule is quenched, and takes out sample, with being dried after alcohol washes, for future use.
5. dumbbell shaped based bulk metallic glasses sample according to claim 1 preparation method it is characterised in that：Step
In three, the original size of described quartz ampoule is：1 centimetre of diameter, 1 millimeter of wall thickness.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756645A (en) * | 2017-02-28 | 2017-05-31 | 深圳市锆安材料科技有限公司 | A kind of inexpensive Fe-based amorphous alloy part preparation technology and Fe-based amorphous alloy part |
| CN109930086A (en) * | 2019-03-04 | 2019-06-25 | 新疆大学 | A kind of iron-base block amorphous state alloy and preparation method thereof with high corrosion resistance |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103757450A (en) * | 2014-01-24 | 2014-04-30 | 新疆大学 | Preparation method of iron-based bulk amorphous alloy with high saturation magnetization |
| CN105586548A (en) * | 2016-02-03 | 2016-05-18 | 北京科技大学 | Massive iron base amorphous alloy with both high strength and high plasticity and preparation method thereof |
-
2016
- 2016-09-30 CN CN201610871540.6A patent/CN106435407B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103757450A (en) * | 2014-01-24 | 2014-04-30 | 新疆大学 | Preparation method of iron-based bulk amorphous alloy with high saturation magnetization |
| CN105586548A (en) * | 2016-02-03 | 2016-05-18 | 北京科技大学 | Massive iron base amorphous alloy with both high strength and high plasticity and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756645A (en) * | 2017-02-28 | 2017-05-31 | 深圳市锆安材料科技有限公司 | A kind of inexpensive Fe-based amorphous alloy part preparation technology and Fe-based amorphous alloy part |
| CN106756645B (en) * | 2017-02-28 | 2018-07-24 | 深圳市锆安材料科技有限公司 | A kind of low cost Fe-based amorphous alloy part preparation process and Fe-based amorphous alloy part |
| CN109930086A (en) * | 2019-03-04 | 2019-06-25 | 新疆大学 | A kind of iron-base block amorphous state alloy and preparation method thereof with high corrosion resistance |
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