CN107473237A - A kind of preparation method of binary tungsten boride superhard material - Google Patents
A kind of preparation method of binary tungsten boride superhard material Download PDFInfo
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- CN107473237A CN107473237A CN201710736601.2A CN201710736601A CN107473237A CN 107473237 A CN107473237 A CN 107473237A CN 201710736601 A CN201710736601 A CN 201710736601A CN 107473237 A CN107473237 A CN 107473237A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/04—Metal borides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses a kind of preparation method of binary tungsten boride superhard material; it is to use machine-alloying; utilize high-energy ball milling; under argon atmosphere; wolfram diboride powder using high purity tungsten and boron powder as raw material direct synthetic powder state at room temperature; then the powder of synthesis is heat-treated, four tungsten boride materials is prepared.The preparation process of the present invention is easy, and controllability is strong, and sintering stage uses atmosphere sintering, and other particular/special requirements are had no to equipment, and universality is strong.
Description
Technical field
The present invention relates to inorganic non-metallic superhard material field, more particularly to a kind of system of binary tungsten boride superhard material
Preparation Method.
Background technology
Superhard material (Hv>40GPa) because it has high hardness and intensity, good wearability, surface stability etc. excellent
It is benign to be widely used in the fields such as machining instrument, wear-resistant coating and grinding-material.According to described in document, WB4In 0.49N
Vickers hardness under load is 43.3 ± 2.9GPa, belongs to superhard material category；Meanwhile WB4There is the height of W-B based compounds again
Fusing point, high rigidity, high conductivity and to excellent properties such as the highly corrosion resistant of different type medium and inoxidizability.Therefore,
Study WB4Preparation there is very high scientific research and practical value.
At present, WB4Preparation mainly use arc melting method, this method mainly using electric energy between electrode with being smelted thing
Between produce electric arc carry out smelting metal.But due to low more of the steaming pressure ratio magnesium-yttrium-transition metal of boron, it is easy in fusion process
Cause the volatilization of boron element and be difficult to obtain desired product；In addition, the vacuum and cooling velocity in arc-melting furnace also can shadows
Ring the quality of product.
The content of the invention
It is an object of the invention to overcome shortcoming present in prior art, there is provided a kind of product quality is high, it is environment-friendly,
Cost is low, the simple binary tungsten boride superhard material of technique.
Another object of the present invention is to provide a kind of preparation method of the above-mentioned superhard material of binary tungsten boride.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of binary tungsten boride superhard material, is to use machine-alloying, using high-energy ball milling, in argon
Under gas shielded atmosphere, the wolfram diboride powder using high purity tungsten (W) powder and boron (B) powder as raw material direct synthetic powder state at room temperature
End, then the powder of synthesis is heat-treated, four tungsten boride materials are prepared.
The preparation method of the binary tungsten boride superhard material, specifically includes following step：
(1) tungsten powder and boron amorphous powder are mixed, using high-energy ball milling equipment, using WC ball grinders and abrading-ball as ball-milling medium,
High-energy ball milling is carried out in argon atmosphere and at room temperature, synthesizes wolfram diboride powder；
(2) wolfram diboride powder is pressed into piece, by isostatic cool pressing pre-molding, obtains wolfram diboride tabletting；
(3) wolfram diboride tabletting is sintered at 1100 DEG C~1400 DEG C under argon gas protection, four boronations is prepared
Tungsten material.
In step (1), the time of ball milling is 40~80h；The material of the abrading-ball is tungsten carbide, the abrading-ball it is a diameter of
6.35~11.20mm, preferably 11.20mm；The mol ratio of the tungsten powder and boron amorphous powder is 1：4.5~12, preferably tungsten powder and non-
The mol ratio of brilliant boron powder is 1：4.5~5.
In step (1), the mass ratio of the gross mass and abrading-ball of the tungsten powder and boron amorphous powder is 1：(4~6)；It is it is preferred that described
The mass ratio of the gross mass and abrading-ball of tungsten powder and boron amorphous powder is 1：4.
In step (2), the pressure of the precompressed is 150~250MPa.
In step (3), the time of the sintering is 1~2h of insulation.
The binary tungsten boride superhard material, is prepared by above-mentioned method.
The binary tungsten boride superhard material, applied to high temperature corrosion-resisting electrode material, cutting tool, crucible and melt
The fields such as casting mould.
The present invention has the following advantages that compared with prior art and effect：
(1) present invention is by controlling B content in raw material proportioning or using B volatilizations under powder embedded sintering method solution high temperature to cause
The problem of can not generating target product, can directly synthesizes wolfram diboride powder at normal temperatures and pressures, at ambient pressure can
So that four fine and close tungsten boride superhard materials are made, its preparation process is easier, and controllability is stronger.
(2) four tungsten boride superhard materials prepared by the present invention have higher purity, and it can be steady in 1400 DEG C of temperature below
It is fixed to exist；It can be used for the fields such as high temperature corrosion-resisting electrode material, cutting tool, crucible and fusion casting die.
(3) sintering stage of the present invention uses atmosphere sintering, and other particular/special requirements are had no to equipment, and universality is stronger, simultaneously
The control to whole technical process can be made easier.
Brief description of the drawings
Fig. 1 is the XRD that powder is made in embodiment 1-6：
(a) powder for being ball milling 20h in embodiment 1；(b) powder for being ball milling 24h in embodiment 2；(c) it is embodiment 3
Middle ball milling 28h powder；(d) powder for being ball milling 32h in embodiment 4；(e) powder for being ball milling 36h in embodiment 5；(f) it is
Ball milling 40h powder in embodiment 6.
Fig. 2 is the XRD comparison diagrams that powder is made in embodiment 6-10：
(a) powder for being ball milling 40h in embodiment 6；(b) powder for being ball milling 50h in embodiment 7；(c) it is embodiment 8
Middle ball milling 60h powder；(d) powder for being ball milling 70h in embodiment 9；(e) powder for being ball milling 80h in embodiment 10.
Fig. 3 is powder (40h) made from embodiment 6 respectively through 1100 DEG C, 1200 DEG C, 1300 DEG C and 1400 DEG C insulation 1h
XRD：
(a) it is the sample through 1100 DEG C of heat treatment in embodiment 11；(b) it is the sample through 1200 DEG C of heat treatment in embodiment 12
Product；(c) it is the sample through 1300 DEG C of heat treatment in embodiment 13；(d) it is the sample through 1400 DEG C of heat treatment in embodiment 14.
Fig. 4 is the XRD that powder is made in embodiment 15, embodiment 16 and embodiment 17：
(a) it is the sample through 1200 DEG C of heat treatment in embodiment 15；(b) it is the sample through 1300 DEG C of heat treatment in embodiment 16
Product；(c) it is the sample through 1400 DEG C of heat treatment in embodiment 17
Fig. 5 is that powder (40h) made from embodiment 6 is not thermally treated and obtained through 1200 DEG C and 1300 DEG C heat treatments respectively
Sample be ground into the SEM photograph of powder：
(a), (b) is the SEM figures of ball milling 40h powder in embodiment 6；(c), (d) is through 1200 DEG C of heat in embodiment 12
The SEM figures that the sample of processing is pulverized；(e), (f) is that the sample through 1300 DEG C of heat treatments in embodiment 13 is pulverized
SEM schemes.
Embodiment
Further detailed description is done to the present invention with reference to embodiment, but the implementation of the present invention is not limited to this.
Unless otherwise specified, the conventional meanses that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagent, method and apparatus.
Equipment used in machine-alloying can be high energy ball mill, vibrator, planetary ball mill, field auxiliary ball
Grinding machine, plasma auxiliary high-energy ball mill etc..Using high energy ball mill (SPEX companies of U.S. model in following examples
For 8000M).For its purity of the tungsten powder used in following examples for 99.95%, the purity of boron amorphous powder is 99.99%, is purchased from city
.
Embodiment 1
(1) ball milling is carried out using high energy ball mill, in the glove box full of argon gas, by high-purity tungsten powder (W) and boron powder
(B) stoichiometrically 1：5 mixes, add the matter of tungsten carbide milling balls six, size 11.20mm, ball and mixed-powder
The ratio between amount is 4:1.
(2) the tungsten-carbide ball grinding jar equipped with powder and abrading-ball is fixed on high energy ball mill.20min is shut down per ball milling 1h
(preventing engine overheat), obtain wolfram diboride powder.
(3) Ball-milling Time is 20h.
Embodiment 2
Difference from Example 1 is, Ball-milling Time 24h, the other the same as in Example 1.
Embodiment 3
Difference from Example 1 is, Ball-milling Time 28h, the other the same as in Example 1.
Embodiment 4
Difference from Example 1 is, Ball-milling Time 32h, the other the same as in Example 1.
Embodiment 5
Difference from Example 1 is, Ball-milling Time 36h, the other the same as in Example 1.
Embodiment 6
Difference from Example 1 is, Ball-milling Time 40h, the other the same as in Example 1.
Fig. 1 is the XRD of wolfram diboride powder made from embodiment 1-6.From figure 1 it appears that do not have during ball milling 20h
Generate any tungsten boride；With the increase of Ball-milling Time, the content of tungsten (W) gradually decreases in powder, wolfram diboride (WB2)
Content gradually increase；During to 40h, tungsten is substantially all to be converted into wolfram diboride (WB2)。
Embodiment 7
Difference from Example 1 is, Ball-milling Time 50h, the other the same as in Example 1.
Embodiment 8
Difference from Example 1 is, Ball-milling Time 60h, the other the same as in Example 1.
Embodiment 9
Difference from Example 1 is, Ball-milling Time 70h, the other the same as in Example 1.
Embodiment 10
Difference from Example 1 is, Ball-milling Time 80h, the other the same as in Example 1.
Fig. 2 is the XRD of wolfram diboride powder made from embodiment 7-10.From figure 2 it can be seen that in ball milling 40-50h
During, very short and small W peaks fade away during 40h, invisible during 50h, illustrate that W has completely reacted；In ball
During grinding 50-80h, each peak does not have any change, product WB2, additionally containing unreacted B.
Embodiment 11
The wolfram diboride powder about 2-4g that Example 6 obtains, thin slice is pressed into Φ 12mm moulds, then passes through 250MPa's
Isostatic cool pressing pre-molding；Then again in tube furnace and under argon gas atmosphere protection, and 2h densified sintering products are incubated at 1100 DEG C,
Obtain four tungsten borides.
Embodiment 12
It is with the difference of embodiment 11, heat treatment temperature is 1200 DEG C, the other the same as in Example 11.
Embodiment 13
It is with the difference of embodiment 11, heat treatment temperature is 1300 DEG C, the other the same as in Example 11.
Embodiment 14
It is with the difference of embodiment 11, heat treatment temperature is 1400 DEG C, the other the same as in Example 11.
Fig. 3 is powder (40h) made from embodiment 6 respectively through 1100 DEG C, 1200 DEG C, 1300 DEG C and 1400 DEG C insulation 1h
XRD.Wherein, (a) is the sample through 1100 DEG C of heat treatment in embodiment 11；(b) it is through 1200 DEG C of heat treatments in embodiment 12
Sample；(c) it is the sample through 1300 DEG C of heat treatment in embodiment 13；(d) it is the sample through 1400 DEG C of heat treatment in embodiment 14
Product.It can be seen that the product of 1100 DEG C and 1200 DEG C heat treatments is all WB4, the production of 1300 DEG C and 1400 DEG C heat treatment
Thing is all WB2.But 1100 DEG C and 1200 DEG C of contrast, it can be seen that WB at 1200 DEG C4Diffraction maximum showed increased, and peak is narrower
Narrow elongated, when illustrating 1100 DEG C and unreacted is complete, and crystallinity is also not so good as 1200 DEG C.1300 DEG C and 1400 DEG C do not have substantially
What difference.But compare with 1200 DEG C, product completely become, by WB4Become WB2, illustrate WB4When being incubated 2h for 1300 DEG C
Time is decomposed.
Embodiment 15
(1) ball milling is carried out using high energy ball mill, in the glove box full of argon gas, by high-purity tungsten powder (W) and boron powder
(B) stoichiometrically 1：8 mixes, add the matter of tungsten carbide milling balls six, size 11.20mm, ball and mixed-powder
The ratio between amount is 4:1.
(2) the tungsten-carbide ball grinding jar equipped with powder and abrading-ball is fixed on high energy ball mill.20min is shut down per ball milling 1h
(preventing engine overheat), obtain wolfram diboride powder.
(3) Ball-milling Time is 65h.
(4) powder obtained after ball milling 65h about 2-4g is taken, is pressed into thin slice with Φ 12mm mould, then pass through 250MPa's
Isostatic cool pressing pre-molding；
(5) in tube furnace, under argon gas atmosphere protection, and 2h densified sintering products are incubated at 1200 DEG C, obtain four tungsten borides.
Embodiment 16
With being for the difference of embodiment 15, heat treatment temperature is 1300 DEG C, the other the same as in Example 15.
Embodiment 17
With being for the difference of embodiment 15, heat treatment temperature is 1400 DEG C, the other the same as in Example 15.
Fig. 4 is the XRD of the powder obtained by embodiment 15-17.Wherein, (a) is through 1200 DEG C of heat treatments in embodiment 15
Sample；(b) it is the sample through 1300 DEG C of heat treatment in embodiment 16；(c) it is the sample through 1400 DEG C of heat treatment in embodiment 17
Product.It can be seen that the product of 1200 DEG C and 1300 DEG C heat treatments is all WB4, the product major part of 1400 DEG C of heat treatment
All it is WB4。
Fig. 5 is that powder (40h) made from embodiment 6 is not thermally treated and obtained through 1200 DEG C and 1300 DEG C heat treatments respectively
Sample be ground into the SEM photograph of powder.Wherein (a), (b) are the SEM photographs of not thermally treated sample powder；(c)、(d)
It is the SEM photograph of 1200 DEG C of heat treatment gained sample powders；(e), (f) is that the SEM of 1300 DEG C of heat treatment gained sample powders shines
Piece.Powder can be milled to Nano grade from (a), (b) it can be seen from the figure that ball milling.Contrast (a), (b) and (e), (f) can be with
Find out, the WB of ball milling generation2Crystallite dimension be less than 1300 DEG C heat treatment generation WB2, illustrate that heat treatment can promote crystal grain to grow
Greatly.And (c), (d) are then 1200 DEG C of WB generated after being heat-treated4Microscopic appearance.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine and simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of binary tungsten boride superhard material, it is characterised in that comprise the steps：
(1) tungsten powder and boron amorphous powder are mixed, using high-energy ball milling equipment, using WC ball grinders and abrading-ball as ball-milling medium, in argon
Gas shielded atmosphere and high-energy ball milling is carried out at room temperature, synthesize wolfram diboride powder；
(2) wolfram diboride powder is pressed into piece, by isostatic cool pressing pre-molding, obtains wolfram diboride tabletting；
(3) wolfram diboride tabletting is sintered at 1100 DEG C~1400 DEG C under argon gas protection, four tungsten boride materials is prepared
Material.
2. the preparation method of binary tungsten boride superhard material according to claim 1, it is characterised in that：In step (1),
The time of ball milling is 40~80h.
3. the preparation method of binary tungsten boride superhard material according to claim 1, it is characterised in that：The abrading-ball
Material is tungsten carbide, a diameter of 6.35~11.20mm of abrading-ball.
4. the preparation method of binary tungsten boride superhard material according to claim 1, it is characterised in that：The tungsten powder and
The mol ratio of boron amorphous powder is 1：4.5~12.
5. the preparation method of binary tungsten boride superhard material according to claim 1, it is characterised in that：In step (1),
The mass ratio of the gross mass and abrading-ball of the tungsten powder and boron amorphous powder is 1：(4~6).
6. the preparation method of binary tungsten boride superhard material according to claim 1, it is characterised in that：In step (2),
The pressure of the precompressed is 150~250MPa.
7. the preparation method of binary tungsten boride superhard material according to claim 1, it is characterised in that：In step (3),
The time of the sintering is 1~2h of insulation.
A kind of 8. binary tungsten boride superhard material, it is characterised in that：It is to use side according to any one of claims 1 to 7
Method is prepared.
A kind of 9. purposes of the binary tungsten boride superhard material described in claim 8, it is characterised in that：Applied to high temperature corrosion resistant
Lose electrode material, cutting tool, crucible and fusion casting die field.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108557834A (en) * | 2018-05-15 | 2018-09-21 | 广东工业大学 | A kind of preparation method of four tungsten boride superhard materials of chromium doping |
| CN108726526A (en) * | 2018-06-04 | 2018-11-02 | 广东工业大学 | A kind of preparation method of four tungsten boride materials of rhenium doping |
| CN109896861A (en) * | 2019-04-11 | 2019-06-18 | 哈尔滨工业大学 | A kind of high-purity, the small grain size hafnium boride raw powder's production technology of resistance to ablation |
| RU2698827C1 (en) * | 2018-08-01 | 2019-08-30 | Общество с ограниченной ответственностью "Газпромнефть Научно-Технический Центр" (ООО "Газпромнефть НТЦ") | Method of producing superhard material and superhard material based on tungsten pentaboride |
| CN111437841A (en) * | 2020-05-15 | 2020-07-24 | 山西大学 | Tungsten telluride-tungsten boride heterojunction electrocatalyst and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108557834A (en) * | 2018-05-15 | 2018-09-21 | 广东工业大学 | A kind of preparation method of four tungsten boride superhard materials of chromium doping |
| CN108726526A (en) * | 2018-06-04 | 2018-11-02 | 广东工业大学 | A kind of preparation method of four tungsten boride materials of rhenium doping |
| WO2019233076A1 (en) * | 2018-06-04 | 2019-12-12 | 广东工业大学 | Preparation method for rhenium-doped tungsten tetraboride material |
| RU2698827C1 (en) * | 2018-08-01 | 2019-08-30 | Общество с ограниченной ответственностью "Газпромнефть Научно-Технический Центр" (ООО "Газпромнефть НТЦ") | Method of producing superhard material and superhard material based on tungsten pentaboride |
| WO2020027688A1 (en) * | 2018-08-01 | 2020-02-06 | Obschestvo S Ogranichennoi Otvetstvennostyu "Gaspromneft Nauchno-Tehnichesky Tsentr" (Ooo "Gaspromneft Ntc") | A method of production of a superhard material and superhard material based on tungsten pentaboride |
| CN109896861A (en) * | 2019-04-11 | 2019-06-18 | 哈尔滨工业大学 | A kind of high-purity, the small grain size hafnium boride raw powder's production technology of resistance to ablation |
| CN111437841A (en) * | 2020-05-15 | 2020-07-24 | 山西大学 | Tungsten telluride-tungsten boride heterojunction electrocatalyst and preparation method and application thereof |
| CN111437841B (en) * | 2020-05-15 | 2023-03-24 | 山西大学 | Tungsten telluride-tungsten boride heterojunction electrocatalyst and preparation method and application thereof |
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