CN107140987A - A kind of Os2B3Hard material and its preparation and application - Google Patents
A kind of Os2B3Hard material and its preparation and application Download PDFInfo
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Abstract
The invention belongs to inorganic non-metallic Hard Materials On Wed, more particularly to a kind of Os2B3Hard material and its preparation method and application.This method is to use mechanochemical reaction, and using high-energy ball milling equipment, using high-purity Os powder and B powder as raw material, Os is synthesized at room temperature2B3Powder；Then high temperature sintering technique is utilized, by the Os of synthesis under argon atmosphere2B3Powder carries out densification sintering, obtains high fine and close, high rigidity block materials.The present invention has synthesized Os at room temperature2B3Powder, and prepare the Os of the hexagonal structure with high-temperature stability2B3Block materials.Os prepared by the present invention2B3Material can be used for cutting tool, the industrial circle such as machine-building, space flight and aviation and automobile.
Description
Technical field
The invention belongs to inorganic non-metallic Hard Materials On Wed, more particularly to a kind of Os2B3Hard material and its preparation and should
With.
Background technology
Superhard material is due to good characteristics such as high rigidity, good wearability and chemical stabilities, being widely used
In various fields such as machine-building, building, space flight and aviation and automobiles.Industrial wide variety of superhard material is mainly gold at present
Hard rock and cubic boron nitride.However, diamond and cubic boron are required under conditions of HTHP synthesizing.Therefore
Need to work out a kind of novel superhard material that can be synthesized under low temperature or normal temperature, to reduce its production cost.
Transition metal boride because it has high rigidity, high bulk modulus, high mechanical properties and high heat endurance and it is standby
It is concerned, what is more important its may be synthesized under low temperature or normal temperature.The transition metal boride of existing research institute's report is main
There is the boride of osmium (Os), rhenium (Re), tungsten (W), iridium (Ir) and ruthenium (Ru).In these transition metals, osmium (Os) has
Highest Valence Electron Density and bulk modulus, and can be with boron (B) formation Os-B and B-B covalent bonds.It is reported that OsB2Vickers it is hard
Degree can reach 37Gpa, and bulk modulus is between 365-395Gpa, the bulk modulus (440Gpa) of its value closely diamond.
But OsB2It is a kind of extremely brittle material, and easy undergo phase transition influences its structure and mechanical property under conditions of high temperature.Os2B3
It is also a kind of hard material in theory and its toughness is better than OsB2。
The content of the invention
In order to overcome the deficiencies in the prior art and shortcoming, primary and foremost purpose of the invention is to provide a kind of Os2B3Firmly
The preparation method of material, preparation process is simple and easy to apply.
It is still another object of the present invention to provide the Os that a kind of above-mentioned preparation method is obtained2B3Hard material, the material has
The excellent physical and chemical performances such as high rigidity, high intensity, wear-resistant and chemical property stabilization.
A further object of the present invention is to provide above-mentioned Os2B3The application of hard material.
The object of the invention is achieved through the following technical solutions：
A kind of Os2B3The preparation method of hard material, comprises the following steps：
(1) mechanochemical reaction is used, under an inert gas, material powder is synthesized by Os by ball mill at room temperature2B3Powder
End；Material powder includes mol ratio 3:2 ＜ B：Os ＜ 5:2；
(2) to the Os of synthesis2B3Powder is granulated, and adds PVA or PVB binding agents thereto, is carried out in a vacuum furnace
Dumping processing, dump temperature is controlled between 400 DEG C -600 DEG C；The addition of the PVA or PVB binding agents is Os2B3Powder matter
The 3% of amount；
(3) under an inert gas, powder is densified using sintering process, obtains Os2B3Hard material.
It is 2 that step (1) described material powder, which includes mol ratio,:1 boron and osmium.
Step (1) described ball mill is planetary high-energy ball mill.When using planetary high-energy ball mill, the synthesis
During using tungsten carbide as ball-milling medium, ball material mass ratio is controlled 4:1.
Step (1) is described to synthesize Os at room temperature by ball mill2B3Powder, its principle is that material powder leads at room temperature
Cross mechanical energy and directly react generation.
Step (1) described Os2B3Powder principal phase is the Os with hexagonal structure2B3。
Step (3) described sintering process is conventional sintering technique or field assisted sintering technique.
Step (3) the conventional sintering technique is hot pressed sintering or atmosphere sintering；The field assisted sintering technique is electric discharge
Plasma agglomeration or microwave sintering.
Step (3) described sintering temperature is 1500-1800 DEG C, preferably 1600-1700 DEG C.
A kind of Os obtained according to above-mentioned preparation method2B3Hard material, the Os2B3The Vickers hardness of hard material reaches
More than 2693Hv.
Above-mentioned Os2B3Hard material is applied to cutting tool and its related industrial fields, is particularly suitable for use in containing ferrous metal
High-speed dry cutting field.
First difficult point that the present invention is intended to solve be, synthesizes that purity is higher, Boron contents are few using mechanochemical reaction or not
The Os with hexagonal structure of boracic2B3Powder；
Second difficult point that the present invention is intended to solve be, the Os of the hexagonal structure of preparation2B3, do not occur at a sintering temperature to
Low boride (OsB1.1) decomposition；
The 3rd difficult point that the present invention is intended to solve is to be prepared using rational sintering process fine and close, without sintering aid
Os2B3Block materials；Described Os2B3Densification process, block materials composition, structure and consistency etc. by sintering process side
Method and sintering parameter control；
The 4th difficult point that the present invention is intended to solve is, to the Os of synthesis2B33% PVA or PVB are added in powder to be subtracted
Lack its lamination in pre-molding.
The 5th difficult point that the present invention is intended to solve is that the block after cold isostatic compaction is carried out at dumping in a vacuum furnace
Reason, can cross the influence for reducing PVA and PVB to block materials performance.
The Os of described use mechanochemical reaction synthesis2B3Main component be the Os with hexagonal structure2B3, Ke Nenghan
There is a certain amount of residual boron.
The present invention has the advantages that to protrude as follows and beneficial effect compared with prior art：(1) traditional superhard material Buddha's warrior attendant
The synthesis of stone and cubic boron nitride needs the conditions such as HTHP.Diamond is easily oxidized at 800 DEG C, and can not process iron content
Class workpiece.The sedimentation rate of cubic boron nitride is low, and depositing temperature is high, and always is difficult to disappear containing some in cubic boron nitride film
H-BN or amorphous BN compositions for removing etc. influence its performance.The Os that this research institute obtains2B3Its purity of material is higher, Boron contents are few or
Person's not boracic, and it has the good characteristics such as higher hardness and chemical stability.(2) it is traditional to prepare transition metal osmium boride
Method have direct reaction sintering, solid-state cementation and electric arc melting etc., and these methods need to carry out under conditions of high temperature and
Cycle is longer, these increased the ultimate cost of product, its unfavorable application industrially.The present invention technical characterstic be,
Using the method for mechanical alloying high-energy ball milling synthesize that purity is higher, Boron contents are few at room temperature, at a normal or boracic does not have
The Os of hexagonal structure2B3Powder, its process is simple and easy to apply.By obtaining the higher block materials of consistency without pressure atmosphere sintering, and
Do not occur in sintering process higher to the transformation purity of low boride.
Brief description of the drawings
Fig. 1 is the XRD spectrum of different Ball-milling Times section, wherein (a) is the XRD spectrum of 4-40h different periods, (b) is (a)
In the partial enlarged drawing of 8-20h different periods, (c) is the partial enlarged drawing of (a) in 16-36h different periods.
Fig. 2 is Os after ball milling 40h2B3SEM the and EDS collection of illustrative plates of powder, wherein (a) is Os after ball milling 40h2B3The SEM of powder
Photo, (b) is Os after (a) ball milling 40h2B3The partial enlargement of the SEM photograph of powder, (c) is Os after ball milling 40h2B3Powder
EDS collection of illustrative plates.
Fig. 3 is Os after ball milling 40h2B3The TEM photos of powder, wherein (a) is Os after ball milling 40h2B3The TEM photos of powder,
(b) it is (a) Os2B3The partial enlargement of the TEM photos of powder, (c) is Os2B3(101) with the interplanar distance of (100) inner plane.
Fig. 4 is Os2B3XPS collection of illustrative plates of the powder after surface etch.
Fig. 5 is Os2B3Powder Os4f (a) and the B1S (matched curves of b electronic shell high-resolution XPS collection of illustrative plates, wherein (a) is
Os2B3The matched curve of powder Os4f (a) electronic shell high-resolution XPS collection of illustrative plates, (b) is Os2B3Powder B1S (b) electronic shell high scores
The matched curve of resolution XPS collection of illustrative plates.
Fig. 6 is Os2B3XRD spectrum after being heat-treated at 800 DEG C and 1000 DEG C.
Fig. 7 is Os2B3XRD spectrum of the powder after 1700 DEG C of atmosphere sinterings.
Fig. 8 is Os after atmosphere sintering2B3Section SEM photograph.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Powder synthesis is carried out using SPEX companies of U.S. model 8000M high energy ball mill.First, full of argon gas
In glove box, by high-purity osmium powder (Os) and boron powder (B) stoichiometrically 1:2 mixes.Tungsten carbide milling balls one used
Totally six, size is 11.20mm, and ball is 4 with mixed-powder mass ratio:1.It will be equipped with the tungsten-carbide ball grinding jar of powder and abrading-ball
It is fixed on high energy ball mill.Ball milling total time is 40h, and 20min (preventing engine overheat) is shut down per ball milling 1h.
Fig. 1 is the XRD spectrum of different ball milling periods.From Fig. 1 (a), with the extension of Ball-milling Time, the peak of osmium (Os) is not
It is disconnected to weaken and peak shape broadens, OsB is detected first after ball milling 2h1.1.Fig. 1 (b) is Fig. 1 (a) partial enlarged drawing, from Fig. 1
(b) understood in, with the extension OsB of Ball-milling Time1.1Peak constantly strengthen, and detect Os after ball milling 12h2B3Peak.Fig. 1 (c)
Partial enlarged drawing for Fig. 1 (a) in the 16-36h periods, can be obtained, Os from Fig. 1 (c)2B3Peak with Ball-milling Time increase without
Disconnected enhancing, is milled to 32h and can't detect Os (osmium) and OsB1.1Peak, its principal phase be Os2B3, continue ball milling peak shape to it basic
Keep constant, its reaction is basically completed after indication ball milling 32h, obtains more pure Os2B3Powder.
Fig. 2 is Os2B3SEM and EDS collection of illustrative plates after ball milling 40h, therefrom it can be seen that due to nanometer powder group caused by cold welding
Poly-, its particle diameter is below 5 μm and in irregular shape.There is a small amount of W (tungsten), C (carbon) and O (oxygen) etc. after ball milling 40h in powder
Impurity element, it is probably introduced by ball-milling medium.Fig. 3 is the TEM diffraction fringes of synthetic powder, it may be determined that ball milling 40h
Resulting powder is the Os of hexagonal structure afterwards2B3。
Fig. 4 is Os2B3XPS collection of illustrative plates after surface etch, is mainly Os as seen from the figure in powder after ball milling 40h
(osmium) and B (boron) both elements, wherein containing a small amount of O (oxygen) element, may during experimental implementation small part product
It there occurs oxidation reaction.
Fig. 5 is Os2B3Powder Os4f (Fig. 5 a) and the high-resolution XPS collection of illustrative plates of B1S (Fig. 5 b) electronic shell matched curve,
Os is understood by Fig. 5 (a) and Fig. 5 (b)2B3In powder between Os (osmium) and B (boron) mainly in the form of Os-B and B-B covalent bonds
In the presence of, and contain a small amount of Os-O and B-O covalent bonds.
Fig. 6 is Os2B3XRD spectrum of the powder after 800 DEG C and 1000 DEG C of two temperature heat treatments.In 800 DEG C, argon gas gas
It is heat-treated under the conditions of a length of 1 hour etc. when atmosphere protection, insulation.As seen from the figure, the powder after 800 DEG C are heat-treated
Its principal phase is still Os compared with not thermally treated2B3.On the premise of other conditions are constant, go out when temperature rises to 1000 DEG C
OsB is showed1.1With Os peak, it can thus be appreciated that there is part Os at a high temperature of 1000 DEG C2B3Powder there occurs to OsB1.1With turning for Os
Become, Os2B3Powder can be stabilized at 800 DEG C.
Fig. 7 is Os2B3XRD spectrum of the powder after 1700 DEG C of atmosphere sinterings, can draw from figure, through 1700 DEG C of atmosphere
Crystallinity and the higher Os2B3 block materials of purity have been obtained after sintering.Its section SEM photograph such as Fig. 8 (a) and (b) are shown,
Sample consistency after sintering is higher, and the plate-like structure of crystal grain, crystallite dimension is larger.The Vickers hardness number of sample is up to
2693Hv0.49N。
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of Os2B3The preparation method of hard material, it is characterised in that comprise the following steps：
(1) mechanochemical reaction is used, under an inert gas, material powder is synthesized by Os by ball mill at room temperature2B3Powder；
Material powder includes mol ratio 3:2 ＜ B：Os ＜ 5:2；
(2) to the Os of synthesis2B3Powder is granulated, and adds PVA or PVB binding agents thereto, and dumping is carried out in a vacuum furnace
Processing, dump temperature is controlled between 400 DEG C -600 DEG C；The addition of the PVA or PVB binding agents is Os2B3Powder quality
3%；
(3) under an inert gas, powder is densified using sintering process, obtains Os2B3Hard material.
2. a kind of Os according to claim 12B3The preparation method of hard material, it is characterised in that：Step (1) described original
It is 2 that feed powder end, which includes mol ratio,:1 boron and osmium.
3. a kind of Os according to claim 12B3The preparation method of hard material, it is characterised in that：Step (1) described ball
Grinding machine is planetary high-energy ball mill；The Os2B3Powder principal phase is the Os with hexagonal structure2B3。
4. a kind of Os according to claim 32B3The preparation method of hard material, it is characterised in that：When using planetary height
During energy ball mill, using tungsten carbide as ball-milling medium during step (1) described synthesis, ball material mass ratio is controlled 4:1.
5. a kind of Os according to claim 12B3The preparation method of hard material, it is characterised in that：Step (3) is described to burn
It is conventional sintering technique or field assisted sintering technique to tie technique.
6. a kind of Os according to claim 52B3The preparation method of hard material, it is characterised in that：Step (3) is described to be passed
Sintering process of uniting is hot pressed sintering or atmosphere sintering；The field assisted sintering technique is discharge plasma sintering or microwave sintering.
7. a kind of Os according to claim 12B3The preparation method of hard material, it is characterised in that：Step (3) is described to burn
Junction temperature is 1500-1800 DEG C.
8. a kind of Os according to claim 72B3The preparation method of hard material, it is characterised in that：The sintering temperature is
1600-1700℃。
9. a kind of Os obtained according to any one of the claim 1-8 preparation methods2B3Hard material, it is characterised in that：It is described
Os2B3The Vickers hardness of hard material reaches more than 2693Hv.
10. Os according to claim 92B3Hard material is applied to cutting tool, machine-building, space flight and aviation and automobile
Deng industrial circle.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108165862A (en) * | 2017-12-11 | 2018-06-15 | 昆明理工大学 | A kind of preparation method of boronation ruthenium superhard alloy |
| CN110526716A (en) * | 2019-08-07 | 2019-12-03 | 广东工业大学 | A kind of boride ceramics and its preparation method and application with high tenacity and high thermal conductivity |
| WO2020103235A1 (en) * | 2018-11-19 | 2020-05-28 | 广东工业大学 | Transition metal boride hard ceramic material, preparation method therefor and application thereof |
| WO2020133585A1 (en) * | 2018-12-27 | 2020-07-02 | 广东工业大学 | Hard transition metal boride material and preparation method therefor |
| CN111560590A (en) * | 2020-05-25 | 2020-08-21 | 北京工业大学 | Preparation method of target material for microwave sintering cathode coating |
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| CN1960834A (en) * | 2004-05-11 | 2007-05-09 | 加利福尼亚大学董事会 | Osmium diboride compounds and their uses |
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| YING LONG ET AL.: "Synthesis of osmium borides by mechanochemical method", 《J AM CERAM SOC.》 * |
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| 曲远方 主编: "《现代陶瓷材料及技术》", 31 May 2008, 华东理工大学出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108165862A (en) * | 2017-12-11 | 2018-06-15 | 昆明理工大学 | A kind of preparation method of boronation ruthenium superhard alloy |
| WO2020103235A1 (en) * | 2018-11-19 | 2020-05-28 | 广东工业大学 | Transition metal boride hard ceramic material, preparation method therefor and application thereof |
| WO2020133585A1 (en) * | 2018-12-27 | 2020-07-02 | 广东工业大学 | Hard transition metal boride material and preparation method therefor |
| CN110526716A (en) * | 2019-08-07 | 2019-12-03 | 广东工业大学 | A kind of boride ceramics and its preparation method and application with high tenacity and high thermal conductivity |
| CN111560590A (en) * | 2020-05-25 | 2020-08-21 | 北京工业大学 | Preparation method of target material for microwave sintering cathode coating |
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