CN105220051B - Mo-Si-B intermetallic compound rod and preparation method thereof - Google Patents
Mo-Si-B intermetallic compound rod and preparation method thereof Download PDFInfo
- Publication number
- CN105220051B CN105220051B CN201510712534.1A CN201510712534A CN105220051B CN 105220051 B CN105220051 B CN 105220051B CN 201510712534 A CN201510712534 A CN 201510712534A CN 105220051 B CN105220051 B CN 105220051B
- Authority
- CN
- China
- Prior art keywords
- melting
- powder
- bar
- intermetallic compound
- less
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The invention discloses a Mo-Si-B intermetallic compound rod. The Mo-Si-B intermetallic compound rod is prepared by the following raw materials in percentage by atom: 8-17% of silicon, 20-30% of boron, and the balance of molybdenum and inevitable impurities. In addition, the invention further discloses a method for preparing the Mo-Si-B intermetallic compound rod; and the method comprises the following steps: (1) raw materials are dried after ball milling to obtain mixed powder; (2) the mixed powder is pressed to form a blank, and is sintered to obtain a Mo-Si-B intermetallic compound sintered body; (3) the Mo-Si-B intermetallic compound sintered body is smelted by an electronic beam to obtain a Mo-Si-B intermetallic compound ingot, and is cut to form a semi-finished rod; and (4) the semi-finished rod is smelted in an electronic beam area to obtain the Mo-Si-B intermetallic compound rod. The Mo-Si-B intermetallic compound rod has the characteristics of high purity and low oxygen mass content, and is broad in application prospect under an ultrahigh-temperature bad extreme environment.
Description
Technical field
The invention belongs to technical field of intermetallic compound, and in particular to a kind of Mo-Si-B intermetallic compounds rod
Material and preparation method thereof.
Background technology
Military power with the U.S. as representative greatly develops advanced theater missile system by the advantage in its science and technology
System (TMD) and NMD (NMD), constitute great threat to other country's ballistic missile.In national defence, China is present
Stern challenge is faced with, either the guided missile of TMD or NMD all to flying with hypersonic maneuver is difficult to intercept, because
We must develop and develop the ballistic missile with stage casing and reentry stage hypersonic maneuver flight performance of a new generation for this.So
And, the realization of these targets is faced with many problems, and one of maximum bottleneck is exactly the development of hyperthermal material.Superhigh temperature
Material plays more and more important effect in national defence and space flight, and we must step up new generation hyperthermal material, be
Realize that these targets accomplish fluently solid foundation.
Mo-Si-B intermetallic compounds have high-melting-point and low-density feature, from room temperature to melting temperature under the conditions of do not have
There is phase transformation, Mo-Si-B intermetallic compounds have complicated crystal structure, possess high elevated temperature strength and high temperature creep
Can, have broad application prospects in the severe extreme environment of superhigh temperature, Mo-Si-B intermetallic compounds be prepare thermal barrier coating and
The important source material of hyperthermal material, but up to the present there is no effective method to prepare Mo in prior art5SiB2Mutually contain
Higher Mo-Si-B intermetallic compounds.
The method for preparing Mo-Si-B intermetallic compounds at present mainly has powder metallurgic method and method of smelting.Using powder
Mo-Si-B intermetallic compounds prepared by metallurgy method inevitably generate the unstable phase of low melting point, even if long by high temperature
The annealing of time is also difficult to eliminate.In addition, Mo-Si-B intermetallic compounds prepared by powder metallurgic method can introduce impurity, oxygen matter
Amount content is high, reduces the mechanical property and antioxygenic property of Mo-Si-B intermetallic compounds.Prepare although with method of smelting
Mo-Si-B intermetallic compounds oxygen mass content it is lower than powder metallurgic method, but still have substantial amounts of transitional face to generate, and
Microstructure is in dendroid, reduces the use temperature and reliability of material.
The content of the invention
The technical problem to be solved is for above-mentioned deficiency of the prior art, there is provided a kind of Mo-Si-B
Intermetallic compound bar, the Mo-Si-B intermetallic compounds bar are to mainly contain Mo5SiB2The rod of intermetallic compound phase
Material, and have purity high and the characteristics of low oxygen mass content, can be used as preparing the painting of superhigh temperature thermal boundary after further crushing powder processed
The raw material of layer and hyperthermal material, has broad application prospects in the severe extreme environment of superhigh temperature.
To solve above-mentioned technical problem, the technical solution used in the present invention is：A kind of Mo-Si-B intermetallic compounds rod
Material, it is characterised in that be made up of the raw material of following atomic percent：Silicon 10%～20%, boron 20%～40%, balance of molybdenum and
Inevitable impurity.
Above-mentioned a kind of Mo-Si-B intermetallic compounds bar, it is characterised in that by the raw material system of following atomic percent
Into：Silicon 13%～17%, boron 25%～35%, balance of molybdenum and inevitable impurity.
Above-mentioned a kind of Mo-Si-B intermetallic compounds bar, it is characterised in that by the raw material system of following atomic percent
Into：Silicon 15%, boron 30%, balance of molybdenum and inevitable impurity.
In addition, present invention also offers a kind of method for preparing above-mentioned Mo-Si-B intermetallic compounds bar, its feature exists
In comprising the following steps：
Step one, silica flour, boron powder and molybdenum powder are placed in ball mill, with dehydrated alcohol as dispersant, in rotating speed are
420rpm～580rpm, ratio of grinding media to material are (10～20):Under conditions of 1, ball milling 28h～42h, is dried after ball milling under vacuum,
Obtain mixed-powder；0.5～1 times for silica flour, boron powder and molybdenum powder quality sum of the volume of the dehydrated alcohol, wherein volume
Unit is mL, and the unit of quality is g；
Step 2, will be mixed-powder described in step one compressing, obtain blank, the blank be placed in into sintering then
In stove, 5 × 10 are less than in vacuum-3It is sintered under conditions of Pa, after furnace cooling, obtains Mo-Si-B intermetallics
Thing sintered body；The temperature of the sintering processes is 1800 DEG C～2000 DEG C, and the time is 2h～3h；
Step 3, the sintered bodies of Mo-Si-B intermetallic compounds described in step 2 are placed in electron beam furnace, true
Reciprocal of duty cycle is less than 5 × 10-4Electronic torch melting 3～6 times under conditions of Pa, obtain Mo-Si-B intermetallic compound ingot castings, so after cooling
The Mo-Si-B intermetallic compounds ingot casting is cut into into semi-finished product bar afterwards；The melting electric current of the electronic torch melting
For 1A～1.2A, melting voltage is 40kV～60kV；
Step 4, semi-finished product bar described in step 3 carried out with polishing remove surface scale, after polishing will it is described partly
Finished product bar is less than 2 × 10 in vacuum-5Electron beam zone melting is carried out under conditions of Pa, Mo-Si-B metals after cooling, are obtained
Between compound bar；The melting electric current of the electron beam zone melting is 0.8A～1A, and melting voltage is 30kV～50kV.
Above-mentioned method, it is characterised in that the quality purity of silica flour described in step one is not less than 99%, the boron powder
Quality purity is not less than 99%, and the quality purity of the molybdenum powder is not less than 99%.
Above-mentioned method, it is characterised in that the temperature of sintering processes described in step 2 is 1850 DEG C～1950 DEG C, time
For 2.2h～2.8h.
Above-mentioned method, it is characterised in that the temperature of the sintering processes is 1900 DEG C, and the time is 2.5h.
Above-mentioned method, it is characterised in that the temperature dried described in step one is 90 DEG C～100 DEG C.
The present invention has advantages below compared with prior art：
1st, the characteristics of Mo-Si-B intermetallic compounds bar of the present invention has purity height and low oxygen mass content, further
Can be as the raw material for preparing superhigh temperature thermal barrier coating and hyperthermal material, in the severe extreme environment of superhigh temperature after crushing powder processed
Under have broad application prospects.
2nd, the present invention adopts ball mill mechanical alloying molybdenum powder, silica flour and boron powder, on the one hand makes three kinds of powder stock mixing
Uniformly, on the other hand can make that three kinds of powder stocks are pre-alloyed, this not only reduces sintering temperature, it is often more important that promote
The reaction of molybdenum powder, silica flour and boron powder generates Mo5SiB2Intermetallic compound phase, using being sintered not only under high vacuum condition
Oxygen mass content in mixed-powder is reduced, while being conducive to molybdenum powder, silica flour and boron powder to react.
3rd, in the present invention technical process of electronic torch melting reduce oxygen in Mo-Si-B intermetallic compound sintered bodies and
The content of other impurities element, is that next step carries out electron beam zone melting and creates condition, the technique of electron beam zone melting
Procedural depth has purified bar, gaseous impurity and other impurities content in the Mo-Si-B intermetallic compound bars for preparing
It is very low.
4th, composition design of the present invention using optimization, it is molten by specific sintering processes+electronic torch melting+E-beam area
The technical process of refining, prepares the Mo-Si-B intermetallic compound bars of perfect crystalline, the Mo-Si-B intermetallic compounds
It is 20ppm～80ppm that the quality purity of bar is 98%～99%, oxygen mass content, being capable of conduct after further crushing powder processed
The raw material of superhigh temperature thermal barrier coating and hyperthermal material is prepared, is had broad application prospects in the severe extreme environment of superhigh temperature.
Below by drawings and Examples, technical scheme is described in further detail.
Description of the drawings
Fig. 1 is the metallograph of Mo-Si-B intermetallic compound bars prepared by the embodiment of the present invention 1.
Fig. 2 is the XRD spectra of Mo-Si-B intermetallic compound bars prepared by the embodiment of the present invention 1.
Specific embodiment
Embodiment 1
The present embodiment Mo-Si-B intermetallic compounds bar is made up of the raw material of following atomic percent：Silicon 15%, boron
30%, balance of molybdenum and inevitable impurity.
The present embodiment prepares the method for Mo-Si-B intermetallic compound bars and comprises the following steps：
Step one, silica flour, boron powder and molybdenum powder are placed in ball mill, with dehydrated alcohol as dispersant, in rotating speed are
500rpm, ratio of grinding media to material are calculated as 15 in mass ratio:Ball milling 35h under conditions of 1, is dried after ball milling under vacuum, is mixed
Powder；The volume of the dehydrated alcohol is 0.7 times of silica flour, boron powder and molybdenum powder quality sum, and the wherein unit of volume is mL, matter
The unit of amount is g；The temperature of the drying is preferably 95 DEG C, it is preferable that the quality purity of the silica flour is not less than 99%, described
The quality purity of boron powder is not less than 99%, and the quality purity of the molybdenum powder is not less than 99%；
Step 2, will be mixed-powder described in step one compressing, obtain blank, the blank be placed in into sintering then
In stove, 5 × 10 are less than in vacuum-3It is sintered under conditions of Pa, after furnace cooling, obtains Mo-Si-B intermetallics
Thing sintered body；The temperature of the sintering processes is 1900 DEG C, and the time is 2.5h, and it is 60mm (length) that the blank is cross sectional dimensions
The strip-shaped blank of × 60mm (width)；
Step 3, the sintered bodies of Mo-Si-B intermetallic compounds described in step 2 are placed in electron beam furnace, true
Reciprocal of duty cycle is less than 5 × 10-4Electronic torch melting 3 times under conditions of Pa, obtain Mo-Si-B intermetallic compound ingot castings, then will be described
Mo-Si-B intermetallic compounds ingot casting is cut into semi-finished product bar, the horizontal stroke of the bar using electric spark wire cutting method
Diameter of section is 30mm, and length is 900mm；The melting electric current of the electronic torch melting is 1.1A, and melting voltage is 50kV；
Step 4, semi-finished product bar described in step 3 carried out with polishing remove surface scale, after polishing will it is described partly
Finished product bar is less than 2 × 10 in vacuum-5Electron beam zone melting is carried out under conditions of Pa, Mo-Si-B metals after cooling, are obtained
Between compound bar；The melting electric current of the electron beam zone melting is 0.9A, and melting voltage is 40kV.
From figure 1 it appears that Mo-Si-B intermetallic compounds bar crystal boundary manufactured in the present embodiment is clear-cut, brilliant
Grain is in the form of a column, without obvious hole, about 520 μm of average grain size, from figure 2 it can be seen that XRD spectra do not occur Mo,
The diffraction maximum of Si and B, shows that Mo, Si and B almost participate in reaction completely, generates and mainly contain Mo5SiB2Intermetallic compound phase
Bar；The quality purity of Mo-Si-B intermetallic compounds bar manufactured in the present embodiment is 99%, and oxygen mass content is
20ppm, can be as the raw material for preparing superhigh temperature thermal barrier coating and hyperthermal material, in superhigh temperature after further crushing powder processed
Severe extreme environment has broad application prospects.
Embodiment 2
The present embodiment Mo-Si-B intermetallic compounds bar is made up of the raw material of following atomic percent：Silicon 17%, boron
35%, balance of molybdenum and inevitable impurity.
The present embodiment prepares the method for Mo-Si-B intermetallic compound bars and comprises the following steps：
Step one, silica flour, boron powder and molybdenum powder are placed in ball mill, with dehydrated alcohol as dispersant, in rotating speed are
420rpm, ratio of grinding media to material are calculated as 20 in mass ratio:Ball milling 42h under conditions of 1, is dried after ball milling under vacuum, is mixed
Powder；The volume of the dehydrated alcohol is 0.5 times of silica flour, boron powder and molybdenum powder quality sum, and the wherein unit of volume is mL, matter
The unit of amount is g；The temperature of the drying is preferably 100 DEG C, it is preferable that the quality purity of the silica flour is not less than 99%, institute
The quality purity of boron powder is stated not less than 99%, the quality purity of the molybdenum powder is not less than 99%；
Step 2, will be mixed-powder described in step one compressing, obtain blank, the blank be placed in into sintering then
In stove, 5 × 10 are less than in vacuum-3It is sintered under conditions of Pa, after furnace cooling, obtains Mo-Si-B intermetallics
Thing sintered body；The temperature of the sintering processes is 1850 DEG C, and the time is 2.8h, and it is 60mm (length) that the blank is cross sectional dimensions
The strip-shaped blank of × 60mm (width)；
Step 3, the sintered bodies of Mo-Si-B intermetallic compounds described in step 2 are placed in electron beam furnace, true
Reciprocal of duty cycle is less than 5 × 10-4Electronic torch melting 4 times under conditions of Pa, obtain Mo-Si-B intermetallic compound ingot castings, then will be described
Mo-Si-B intermetallic compounds ingot casting is cut into semi-finished product bar, the horizontal stroke of the bar using electric spark wire cutting method
Diameter of section is 30mm, and length is 900mm；The melting electric current of the electronic torch melting is 1A, and melting voltage is 40kV；
Step 4, semi-finished product bar described in step 3 carried out with polishing remove surface scale, after polishing will it is described partly
Finished product bar is less than 2 × 10 in vacuum-5Electron beam zone melting is carried out under conditions of Pa, Mo-Si-B metals after cooling, are obtained
Between compound bar；The melting electric current of the electron beam zone melting is 0.8A, and melting voltage is 30kV.
The present embodiment has been prepared and has mainly contained Mo5SiB2The Mo-Si-B intermetallic compound rods of intermetallic compound phase
Material, the Mo-Si-B intermetallic compound bar crystal boundaries are clear-cut, crystal grain is in the form of a column, and without obvious hole, its quality purity is
98.6%, oxygen mass content is 34ppm, can be used as preparation superhigh temperature thermal barrier coating and superhigh temperature material after further crushing powder processed
The raw material of material, has broad application prospects in the severe extreme environment of superhigh temperature.
Embodiment 3
The present embodiment Mo-Si-B intermetallic compounds bar is made up of the raw material of following atomic percent：Silicon 13%, boron
25%, balance of molybdenum and inevitable impurity.
The present embodiment prepares the method for Mo-Si-B intermetallic compound bars and comprises the following steps：
Step one, silica flour, boron powder and molybdenum powder are placed in ball mill, with dehydrated alcohol as dispersant, in rotating speed are
580rpm, ratio of grinding media to material are calculated as 10 in mass ratio:Ball milling 28h under conditions of 1, is dried after ball milling under vacuum, is mixed
Powder；The volume of the dehydrated alcohol be silica flour, boron powder and molybdenum powder quality it is equal, wherein the unit of volume be mL, the list of quality
Position is g；The temperature of the drying is preferably 90 DEG C, it is preferable that the quality purity of the silica flour is not less than 99%, the boron powder
Quality purity is not less than 99%, and the quality purity of the molybdenum powder is not less than 99%；
Step 2, will be mixed-powder described in step one compressing, obtain blank, the blank be placed in into sintering then
In stove, 5 × 10 are less than in vacuum-3It is sintered under conditions of Pa, after furnace cooling, obtains Mo-Si-B intermetallics
Thing sintered body；The temperature of the sintering processes is 1950 DEG C, and the time is 2.2h, and it is 60mm (length) that the blank is cross sectional dimensions
The strip-shaped blank of × 60mm (width)；
Step 3, the sintered bodies of Mo-Si-B intermetallic compounds described in step 2 are placed in electron beam furnace, true
Reciprocal of duty cycle is less than 5 × 10-4Electronic torch melting 5 times under conditions of Pa, obtain Mo-Si-B intermetallic compound ingot castings, then will be described
Mo-Si-B intermetallic compounds ingot casting is cut into semi-finished product bar, the horizontal stroke of the bar using electric spark wire cutting method
Diameter of section is 30mm, and length is 900mm；The melting electric current of the electronic torch melting is 1.2A, and melting voltage is 60kV；
Step 4, to semi-finished product bar described in step 3 carry out polishing remove surface scale, then using anhydrous second
Alcohol is cleaned up, and is placed in the smelting furnace of electro-beam floating zone domain, is less than 2 × 10 in vacuum after polishing cleaning-5Under conditions of Pa
Electron beam zone melting is carried out, Mo-Si-B intermetallic compound bars after cooling, are obtained；The melting of the electron beam zone melting
Electric current is 1A, and melting voltage is 50kV.
The present embodiment has been prepared and has mainly contained Mo5SiB2The Mo-Si-B intermetallic compound rods of intermetallic compound phase
Material, the Mo-Si-B intermetallic compound bar crystal boundaries are clear-cut, crystal grain is in the form of a column, and without obvious hole, its quality purity is
99%, oxygen mass content is 60ppm, can be used as preparation superhigh temperature thermal barrier coating and hyperthermal material after further crushing powder processed
Raw material, have broad application prospects in the severe extreme environment of superhigh temperature.
Embodiment 4
The present embodiment Mo-Si-B intermetallic compounds bar is made up of the raw material of following atomic percent：Silicon 20%, boron
40%, balance of molybdenum and inevitable impurity.
The present embodiment prepares the method for Mo-Si-B intermetallic compound bars and comprises the following steps：
Step one, silica flour, boron powder and molybdenum powder are placed in ball mill, with dehydrated alcohol as dispersant, in rotating speed are
500rpm, ratio of grinding media to material are calculated as 18 in mass ratio:Ball milling 35h under conditions of 1, is dried after ball milling under vacuum, is mixed
Powder；The volume of the dehydrated alcohol be silica flour, boron powder and molybdenum powder quality it is equal, wherein the unit of volume be mL, the list of quality
Position is g；The temperature of the drying is preferably 90 DEG C, it is preferable that the quality purity of the silica flour is not less than 99%, the boron powder
Quality purity is not less than 99%, and the quality purity of the molybdenum powder is not less than 99%；
Step 2, will be mixed-powder described in step one compressing, obtain blank, the blank be placed in into sintering then
In stove, 5 × 10 are less than in vacuum-3It is sintered under conditions of Pa, after furnace cooling, obtains Mo-Si-B intermetallics
Thing sintered body；The temperature of the sintering processes is 1900 DEG C, and the time is 2.5h, and it is 60mm (length) that the blank is cross sectional dimensions
The strip-shaped blank of × 60mm (width)；
Step 3, the sintered bodies of Mo-Si-B intermetallic compounds described in step 2 are placed in electron beam furnace, true
Reciprocal of duty cycle is less than 5 × 10-4Electronic torch melting 6 times under conditions of Pa, obtain Mo-Si-B intermetallic compound ingot castings, then will be described
Mo-Si-B intermetallic compounds ingot casting is cut into semi-finished product bar, the horizontal stroke of the bar using electric spark wire cutting method
Diameter of section is 30mm, and length is 900mm；The melting electric current of the electronic torch melting is 10.5A, and melting voltage is 43kV；
Step 4, semi-finished product bar described in step 3 carried out with polishing remove surface scale, after polishing will it is described partly
Finished product bar is less than 2 × 10 in vacuum-5Electron beam zone melting is carried out under conditions of Pa, Mo-Si-B metals after cooling, are obtained
Between compound bar；The melting electric current of the electron beam zone melting is 0.85A, and melting voltage is 33kV.
The present embodiment has been prepared and has mainly contained Mo5SiB2The Mo-Si-B intermetallic compound rods of intermetallic compound phase
Material, the Mo-Si-B intermetallic compound bar crystal boundaries are clear-cut, crystal grain is in the form of a column, and without obvious hole, its quality purity is
98%, oxygen mass content is 34ppm, can be used as preparation superhigh temperature thermal barrier coating and hyperthermal material after further crushing powder processed
Raw material, have broad application prospects in the severe extreme environment of superhigh temperature.
Embodiment 5
The present embodiment Mo-Si-B intermetallic compounds bar is made up of the raw material of following atomic percent：Silicon 10%, boron
20%, balance of molybdenum and inevitable impurity.
The present embodiment prepares the method for Mo-Si-B intermetallic compound bars and comprises the following steps：
Step one, silica flour, boron powder and molybdenum powder are placed in ball mill, with dehydrated alcohol as dispersant, in rotating speed are
550rpm, ratio of grinding media to material are calculated as 13 in mass ratio:Ball milling 30h under conditions of 1, is dried after ball milling under vacuum, is mixed
Powder；The volume of the dehydrated alcohol be silica flour, boron powder and molybdenum powder quality it is equal, wherein the unit of volume be mL, the list of quality
Position is g；The temperature of the drying is preferably 100 DEG C, it is preferable that the quality purity of the silica flour is not less than 99%, the boron powder
Quality purity be not less than 99%, the quality purity of the molybdenum powder is not less than 99%；
Step 2, will be mixed-powder described in step one compressing, obtain blank, the blank be placed in into sintering then
In stove, 5 × 10 are less than in vacuum-3It is sintered under conditions of Pa, after furnace cooling, obtains Mo-Si-B intermetallics
Thing sintered body；The temperature of the sintering processes be 1800 DEG C, the time is 3h, the blank be cross sectional dimensions be 60mm (length) ×
The strip-shaped blank of 60mm (width)；
Step 3, the sintered bodies of Mo-Si-B intermetallic compounds described in step 2 are placed in electron beam furnace, true
Reciprocal of duty cycle is less than 5 × 10-4Electronic torch melting 5 times under conditions of Pa, obtain Mo-Si-B intermetallic compound ingot castings, then will be described
Mo-Si-B intermetallic compounds ingot casting is cut into semi-finished product bar, the horizontal stroke of the bar using electric spark wire cutting method
Diameter of section is 30mm, and length is 900mm；The melting electric current of the electronic torch melting is 11.5A, and melting voltage is 57kV；
Step 4, semi-finished product bar described in step 3 carried out with polishing remove surface scale, after polishing will it is described partly
Finished product bar is less than 2 × 10 in vacuum-5Electron beam zone melting is carried out under conditions of Pa, Mo-Si-B metals after cooling, are obtained
Between compound bar；The melting electric current of the electron beam zone melting is 0.95A, and melting voltage is 47kV.
The present embodiment has been prepared and has mainly contained Mo5SiB2The Mo-Si-B intermetallic compound rods of intermetallic compound phase
Material, the Mo-Si-B intermetallic compound bar crystal boundaries are clear-cut, crystal grain is in the form of a column, and without obvious hole, its quality purity is
98.5%, oxygen mass content is 80ppm, can be used as preparation superhigh temperature thermal barrier coating and superhigh temperature material after further crushing powder processed
The raw material of material, has broad application prospects in the severe extreme environment of superhigh temperature.
Embodiment 6
The present embodiment Mo-Si-B intermetallic compounds bar is made up of the raw material of following atomic percent：Silicon 14%, boron
26%, balance of molybdenum and inevitable impurity.
The present embodiment prepares the method for Mo-Si-B intermetallic compound bars and comprises the following steps：
Step one, silica flour, boron powder and molybdenum powder are placed in ball mill, with dehydrated alcohol as dispersant, in rotating speed are
480rpm, ratio of grinding media to material are calculated as 14 in mass ratio:Ball milling 40h under conditions of 1, is dried after ball milling under vacuum, is mixed
Powder；The volume of the dehydrated alcohol be silica flour, boron powder and molybdenum powder quality it is equal, wherein the unit of volume be mL, the list of quality
Position is g；The temperature of the drying is preferably 95 DEG C, it is preferable that the quality purity of the silica flour is not less than 99%, the boron powder
Quality purity is not less than 99%, and the quality purity of the molybdenum powder is not less than 99%；
Step 2, will be mixed-powder described in step one compressing, obtain blank, the blank be placed in into sintering then
In stove, 5 × 10 are less than in vacuum-3It is sintered under conditions of Pa, after furnace cooling, obtains Mo-Si-B intermetallics
Thing sintered body；The temperature of the sintering processes be 2000 DEG C, the time is 2h, the blank be cross sectional dimensions be 60mm (length) ×
The strip-shaped blank of 60mm (width)；
Step 3, the sintered bodies of Mo-Si-B intermetallic compounds described in step 2 are placed in electron beam furnace, true
Reciprocal of duty cycle is less than 5 × 10-4Electronic torch melting 5 times under conditions of Pa, obtain Mo-Si-B intermetallic compound ingot castings, then will be described
Mo-Si-B intermetallic compounds ingot casting is cut into semi-finished product bar, the horizontal stroke of the bar using electric spark wire cutting method
Diameter of section is 30mm, and length is 900mm；The melting electric current of the electronic torch melting is 1.2A, and melting voltage is 40kV；
Step 4, semi-finished product bar described in step 3 carried out with polishing remove surface scale, after polishing will it is described partly
Finished product bar is less than 2 × 10 in vacuum-5Electron beam zone melting is carried out under conditions of Pa, Mo-Si-B metals after cooling, are obtained
Between compound bar；The melting electric current of the electron beam zone melting is 0.8A, and melting voltage is 50kV.
The present embodiment has been prepared and has mainly contained Mo5SiB2The Mo-Si-B intermetallic compound rods of intermetallic compound phase
Material, the Mo-Si-B intermetallic compound bar crystal boundaries are clear-cut, crystal grain is in the form of a column, and without obvious hole, its quality purity is
98.9%, oxygen mass content is 39ppm, can be used as preparation superhigh temperature thermal barrier coating and superhigh temperature material after further crushing powder processed
The raw material of material, has broad application prospects in the severe extreme environment of superhigh temperature.
The above, is only presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, every according to the present invention
Any simple modification, change and equivalent structure change that technical spirit is made to above example, still fall within skill of the present invention
In the protection domain of art scheme.
Claims (8)
1. a kind of Mo-Si-B intermetallic compounds bar, it is characterised in that be made up of the raw material of following atomic percent：Silicon
10%～20%, boron 20%～40%, balance of molybdenum and inevitable impurity；
The method for preparing the Mo-Si-B intermetallic compound bars is：
Step one, silica flour, boron powder and molybdenum powder are placed in ball mill, with dehydrated alcohol as dispersant, rotating speed be 420rpm～
580rpm, ratio of grinding media to material are (10～20):Under conditions of 1, ball milling 28h～42h, dries after ball milling under vacuum, is mixed
Powder；The volume of the dehydrated alcohol is 0.5～1 times of silica flour, boron powder and molybdenum powder quality sum, and the unit of wherein volume is
ML, the unit of quality is g；
Step 2, will be mixed-powder described in step one compressing, obtain blank, the blank be placed in into sintering furnace then
In, 5 × 10 are less than in vacuum-3It is sintered under conditions of Pa, after furnace cooling, obtains Mo-Si-B intermetallic compounds
Sintered body；The temperature of the sintering processes is 1800 DEG C～2000 DEG C, and the time is 2h～3h；
Step 3, the sintered bodies of Mo-Si-B intermetallic compounds described in step 2 are placed in electron beam furnace, in vacuum
Less than 5 × 10-4Electronic torch melting 3～6 times under conditions of Pa, obtain Mo-Si-B intermetallic compound ingot castings after cooling, then will
The Mo-Si-B intermetallic compounds ingot casting is cut into semi-finished product bar；The melting electric current of the electronic torch melting is 1A
～1.2A, melting voltage are 40kV～60kV；
Step 4, to semi-finished product bar described in step 3 carry out polishing remove surface scale, by the semi-finished product after polishing
Bar is less than 2 × 10 in vacuum-5Electron beam zone melting is carried out under conditions of Pa, obtains changing between Mo-Si-B metals after cooling
Compound bar；The melting electric current of the electron beam zone melting is 0.8A～1A, and melting voltage is 30kV～50kV.
2. according to a kind of Mo-Si-B intermetallic compounds bar described in claim 1, it is characterised in that by following atom hundred
The raw material of ratio is divided to make：Silicon 13%～17%, boron 25%～35%, balance of molybdenum and inevitable impurity.
3. according to a kind of Mo-Si-B intermetallic compounds bar described in claim 2, it is characterised in that by following atom hundred
The raw material of ratio is divided to make：Silicon 15%, boron 30%, balance of molybdenum and inevitable impurity.
4. a kind of method for preparing the Mo-Si-B intermetallic compounds bar as described in any claim in claims 1 to 3,
Characterized in that, comprising the following steps：
Step one, silica flour, boron powder and molybdenum powder are placed in ball mill, with dehydrated alcohol as dispersant, rotating speed be 420rpm～
580rpm, ratio of grinding media to material are (10～20):Under conditions of 1, ball milling 28h～42h, dries after ball milling under vacuum, is mixed
Powder；The volume of the dehydrated alcohol is 0.5～1 times of silica flour, boron powder and molybdenum powder quality sum, and the unit of wherein volume is
ML, the unit of quality is g；
Step 2, will be mixed-powder described in step one compressing, obtain blank, the blank be placed in into sintering furnace then
In, 5 × 10 are less than in vacuum-3It is sintered under conditions of Pa, after furnace cooling, obtains Mo-Si-B intermetallic compounds
Sintered body；The temperature of the sintering processes is 1800 DEG C～2000 DEG C, and the time is 2h～3h；
Step 3, the sintered bodies of Mo-Si-B intermetallic compounds described in step 2 are placed in electron beam furnace, in vacuum
Less than 5 × 10-4Electronic torch melting 3～6 times under conditions of Pa, obtain Mo-Si-B intermetallic compound ingot castings after cooling, then will
The Mo-Si-B intermetallic compounds ingot casting is cut into semi-finished product bar；The melting electric current of the electronic torch melting is 1A
～1.2A, melting voltage are 40kV～60kV；
Step 4, to semi-finished product bar described in step 3 carry out polishing remove surface scale, by the semi-finished product after polishing
Bar is less than 2 × 10 in vacuum-5Electron beam zone melting is carried out under conditions of Pa, obtains changing between Mo-Si-B metals after cooling
Compound bar；The melting electric current of the electron beam zone melting is 0.8A～1A, and melting voltage is 30kV～50kV.
5. in accordance with the method for claim 4, it is characterised in that the quality purity of silica flour described in step one is not less than
99%, the quality purity of the boron powder is not less than 99%, and the quality purity of the molybdenum powder is not less than 99%.
6. in accordance with the method for claim 4, it is characterised in that the temperature of sintering processes described in step 2 be 1850 DEG C～
1950 DEG C, the time is 2.2h～2.8h.
7. in accordance with the method for claim 6, it is characterised in that the temperature of the sintering processes is 1900 DEG C, and the time is
2.5h。
8. in accordance with the method for claim 4, it is characterised in that the temperature dried described in step one is 90 DEG C～100 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510712534.1A CN105220051B (en) | 2015-10-28 | 2015-10-28 | Mo-Si-B intermetallic compound rod and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510712534.1A CN105220051B (en) | 2015-10-28 | 2015-10-28 | Mo-Si-B intermetallic compound rod and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105220051A CN105220051A (en) | 2016-01-06 |
| CN105220051B true CN105220051B (en) | 2017-04-12 |
Family
ID=54989315
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510712534.1A Expired - Fee Related CN105220051B (en) | 2015-10-28 | 2015-10-28 | Mo-Si-B intermetallic compound rod and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105220051B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106048488B (en) * | 2016-06-21 | 2019-05-24 | 西安理工大学 | A method of high-temperature oxidation resistant coating is prepared on refractory metal material surface |
| CN108251670B (en) * | 2016-12-28 | 2020-01-10 | 有研工程技术研究院有限公司 | Preparation method of high-temperature-resistant intermetallic compound alloy |
| CN107385367B (en) * | 2017-08-02 | 2018-10-23 | 西北有色金属研究院 | A kind of preparation method of fine grain hypoxemia type Multiphase Mo-Si-B alloys |
| CN108580882B (en) * | 2018-06-20 | 2019-12-17 | 西安琦丰光电科技有限公司 | powder ball-milling mixing method of molybdenum-silicon-boron material for additive manufacturing |
| CN110607562B (en) * | 2019-10-28 | 2021-02-09 | 西北有色金属研究院 | Preparation method of Mo-Nb-W-Zr alloy single crystal bar |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6652674B1 (en) * | 2002-07-19 | 2003-11-25 | United Technologies Corporation | Oxidation resistant molybdenum |
| JP3735717B2 (en) * | 2002-09-24 | 2006-01-18 | 国立大学法人東北大学 | Mo-Si-B alloy |
| AT6955U1 (en) * | 2003-09-19 | 2004-06-25 | Plansee Ag | ODS MOLYBDENUM-SILICON ALLOY BOR |
| CN102424928B (en) * | 2011-12-03 | 2013-07-31 | 西北有色金属研究院 | Mo-Si-B-W multi-phase composite material and preparation method thereof |
| CN103160701A (en) * | 2011-12-09 | 2013-06-19 | 北京有色金属研究总院 | Preparation method for high-temperature-resistant Mo-Si-B alloy |
-
2015
- 2015-10-28 CN CN201510712534.1A patent/CN105220051B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN105220051A (en) | 2016-01-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105220051B (en) | Mo-Si-B intermetallic compound rod and preparation method thereof | |
| CN102717086B (en) | Method for preparing high-niobium titanium-aluminum alloy spherical micro powder in short process | |
| CN102652184B (en) | Magnetic material sputtering target | |
| CN102888531B (en) | Quick-forming component alpha and beta type titan alloy silk material piled up by a kind of 960MPa intensity level electron beam fuse | |
| CN101967582B (en) | Method for smelting molybdenum titanium alloy | |
| JP5807119B2 (en) | Processing method of molybdenum / niobium alloy plate target material | |
| CN109706363B (en) | Eutectic high-entropy alloy and preparation method thereof | |
| CN104674038A (en) | Alloy material with high strength as well as ductility and semi-solid state sintering preparation method and application of alloy material | |
| CN103938102A (en) | Preparation method of iron, chromium and aluminum multielement electrothermal alloy with high resistance | |
| CN113020598B (en) | Selective laser melting formed nickel-based high-temperature alloy and preparation method thereof | |
| CN102776412B (en) | In one, Quick-forming component titanium alloy wire materials piled up by strong high tenacity electron beam fuse | |
| CN106670482A (en) | Preparing method for superfine high-grade spherical GH4133 alloy powder | |
| CN102601367B (en) | The heat treatment method of a kind of radiation or multipole oriental magnetic ring | |
| KR102197604B1 (en) | Titanium-aluminium base alloy for 3d printing having excellent high temperature property and method of manufacturing the same | |
| GB2575005A (en) | A process and method for producing titanium and titanium alloy billets, spherical and non-spherical powder | |
| CN114134385A (en) | Refractory medium-entropy alloy and preparation method thereof | |
| CN105256214B (en) | Nb-Si intermetallic compound bar and preparation method thereof | |
| CN112981180B (en) | Preparation method of medium-density ultrahigh-plasticity nickel-tungsten alloy shaped charge liner material | |
| Chen et al. | Characterization of LaB6–ZrB2 eutectic composite grown by the floating zone method | |
| CN116287913A (en) | Microelement modified aluminum lithium alloy powder for additive manufacturing and preparation method thereof | |
| CN107760952B (en) | A kind of Mo-Si-C alloy bar materials and preparation method thereof | |
| CN107267826A (en) | A kind of modified graphene enhancing magnesium-base metal material and preparation method thereof | |
| CN106834857A (en) | A kind of W WC TiC Hf Co alloy bar materials and preparation method thereof | |
| CN104032152A (en) | Preparation method for Cu-Nb nano-dispersion reinforced copper alloy | |
| CN110343932B (en) | WVTaZrSc refractory high-entropy alloy with high strength and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170412 Termination date: 20211028 |