CN106518076A - Non-pressure synthesis method for Ti2SbP powder material - Google Patents
Non-pressure synthesis method for Ti2SbP powder material Download PDFInfo
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The invention relates to a non-pressure synthesis method for a Ti2SbP powder material. The method comprises the following steps: 1) weighing Ti powder, Sb powder and TiP powder according to a mol ratio of Ti to Sb to TiP of 1: (0.5-1.5): (0.7-2.5) for subsequent usage; 2) uniformly mixing the weighed Ti powder, Sb powder and TiP powder, sealing the obtained mixture in a vacuum quartz tube and carrying out calcining in a muffle furnace, wherein during calcining, temperature is allowed to rise to 800 to 1150 DEG C at a heating rate of 5 to 100 DEG C/min and then the temperature is maintained for 10 to 48 h; and 4) after completion of calcining, turning off a power supply and then carrying out natural cooling so as to obtain the high-purity Ti2SbP powder material. The method provided by the invention is simple in process, low in cost, high in yield and suitable for industrial large-scale production.
Description
Technical field
The invention belongs to advanced ceramics material field, is related to a kind of nothing and is pressed into Ti2The method of SbP powder body materials, especially
It is related to a kind of ceramic layered Ti of novel tertiary2The preparation method of SbP powder body materials.
Background technology
MAX (or Mn+1AXn, n=1,2,3) it is mutually series of ceramic material.The formula and structure of MAX phases be by
M.W.Barsoum[1-3]Definition, M be early stage transition metal, A be mainly III and IV major elements, X be C and N, in periodic chart
M can be formedn+1AXnThe element of phase is as shown in Figure 1.Up to the present, it has been found that compound have nearly 60 kinds.This kind of chemical combination
Thing has six side's layer structures, belongs to P63/ mmc space groups, Mn+1XnLayer is separated by element A layer, as shown in Figure 2[1]。
This special nanometer laminated structure, determines compound while having the premium properties of metal and ceramics：And gold
Category is the same, at normal temperatures, has good heat conductivility and electric conductivity, has relatively low Vickers hardness and higher springform
Amount and modulus of shearing, can carry out machining as graphite, and have plasticity at high temperature as metal；Meanwhile, it has
The performance of ceramic material, has high yield strength, high-melting-point, high thermal stability and good antioxygenic property；More meaningful
It is that they have even better than graphite and MoS2Self-lubricating property.These unique performances so that no matter this kind of material is on basis
Field still all has very big Research Significance in application.MAX phase materials are in medical template, hot pressing cutter and heat-resisting
Applied in terms of material[4-5].In following more technical fields, it may have wide application prospect.
In the periodic table of elements, the new extension for constantly seeking MAX phases is the one side that material worker is keen to.In MAX
In the formula definition of phase, X is C element and N element.Also other elements can be substituted？A.Yakoubi in 2011[6]Pass through
Structure and chemical bonding analysis to material, gives MAX phases researcher one affirmative reply：M2SbP (M=Ti, Zr, Hf) also belongs to
In MAX phases.It has been found that the study on the synthesis of this kind of compound and theoretical research are very rare in literature search.Synthesis is ground
Study carefully aspect, only report is the H.Boller in 1973[7]Element powder is sealed in quartz ampoule, 48 is calcined at 800 DEG C
Hour, after taking-up powder mull in quartz ampoule is again sealed off, calcine 48 hours at 800 DEG C.The document is write with German,
Give Ti2SbP、Zr2SbP and Hf2The cell parameter and diffraction peak of tri- kinds of materials of SbP, but do not provide diffraction pattern
Spectrum, it is impossible to learn the purity of material.Also trial synthesizes Ti with the method to inventor herein2SbP, has obtained this ternary really
Phase, but purity is very low.After this, as the synthetically prepared control difficulty of phosphide is larger, then do not find with regard to
M2SbP is combined to the report of aspect, and the performance study of this kind of material is even more blank.In terms of theoretical research, only report is
Previously mentioned A.Yaoubi in 2011[6]This paper, found by the structure to material and chemical bonding analysis, Ti2SbP
And Zr2The bulk modulus of SbP is identical, but Hf2The bulk modulus of SbP compares Ti2SbP increases by 8.7%；This be due to
After Hf substitutes Ti, the valency electron for filling p-d hydridization bonding states increases caused.The research is to understanding M2The knot of SbP compounds
Structure and chemical bond are extremely important, also have directive significance to compound experiment.
The content of the invention
It is an object of the invention to provide a kind of nothing is pressed into Ti2The method of SbP powder body materials, particularly a kind of new three
The ceramic layered Ti of unit2The preparation method of SbP powder body materials, prepared Ti2SbP powder body has higher purity.
To achieve these goals, the technical scheme is that：A kind of nothing is pressed into Ti2The method of SbP powder body materials,
Characterized in that, methods described comprises the steps：
1) by Ti powder, Sb powder, three kinds of raw materials of TiP powder mol ratio be Ti:Sb:TiP=1：(0.5～1.5)：(0.7～
2.5) Ti powder, Sb powder, TiP powder raw materials, are weighed, it is standby；
2) after Ti powder, Sb powder, TiP mix homogeneously will be weighed, it is sealed in vitreosil pipe, is forged in being put into Muffle furnace
Burn；
3) heating step is：800～1150 DEG C are risen to the heating rate of 5～100 DEG C/min, 10～48 hours are incubated；
4), after the completion of calcining, power off, natural cooling, obtain high-purity Ti 2SbP powder body materials.
Further, the method that described nothing is pressed into Ti2SbP powder body materials, it is characterised in that：Ti powder, Sb powder, TiP
The mol ratio of three kinds of raw materials of powder is Ti:Sb:TiP=1：1.3：1.6.
Further, the method that described nothing is pressed into Ti2SbP powder body materials, it is characterised in that：Ti powder, Sb powder, TiP
The mol ratio of three kinds of raw materials of powder is Ti:Sb:TiP=1：1.2：2.0.
Further, the method that described nothing is pressed into Ti2SbP powder body materials, it is characterised in that：Ti powder, Sb powder, TiP
The mol ratio of three kinds of raw materials of powder is Ti:Sb:TiP=1：0.5：2.5.
Further, the method that described nothing is pressed into Ti2SbP powder body materials, it is characterised in that：Ti powder, Sb powder, TiP
The mol ratio of three kinds of raw materials of powder is Ti:Sb:TiP=1：1.5：0.7.
Further, the method that described nothing is pressed into Ti2SbP powder body materials, it is characterised in that：Ti powder, Sb powder, TiP
The mol ratio of three kinds of raw materials of powder is Ti:Sb:TiP=1：0.8：1.2.
Further, the method that described nothing is pressed into Ti2SbP powder body materials, it is characterised in that：Ti powder, Sb powder, TiP
The mol ratio of three kinds of raw materials of powder is Ti:Sb:TiP=1：1.21：1.51.
The invention has the beneficial effects as follows：
1st, the key factor of product of the present invention is that reactant powder is enclosed within vitreosil pipe, it is therefore prevented that phosphide is waved
Send out.In experiments it is found that, phosphatization titanium can volatilize in heating process, if these volatile matters are allowed to evaporate in air, can be right
Environment causes significant damage, cannot also participate in chemical reaction, it is impossible to obtain the compound that we need to synthesize.
2nd, the present invention prepares Ti using a kind of reaction in-situ2SbP powder body materials, its ultimate principle are using extraneous heating
(heating-up temperature is by 800～1150 DEG C) react the big calorimetric released and Ti, Sb between, raise system temperature, and TiP is dissolved in
In TiSb base fluid bodies, after exothermic reaction terminates, system temperature declines therewith, ternary phase Ti2SbP is separated out.
3rd, the present invention prepares high-purity Ti using fabricated in situ technique2SbP powder body materials, without interface pollution.It is whole to prepare
The raw material that process is selected is simple, takes full advantage of reaction in-situ advantage, and synthesis temperature is low.Present invention process is simple and reliable, into
This low, yield is high.
4th, Ti in product of the invention2The content of SbP can be by internal mark method determination, and its value is up to 96.2%.
Description of the drawings
Fig. 1 be the periodic table of elements in can form Mn+1AXnThe schematic diagram of phase element.
Fig. 2 is Mn+1AXnThe structure diagram of phase.
Fig. 3 is Ti powder, the mol ratio of Sb powder, three kinds of raw materials of TiP powder is Ti:Sb:TiP=1：(0.5～1.5)：(0.7～
2.5) the in-situ hot pressing technique sintering Ti in the range of2The X ray diffracting spectrum of SbP samples.By analysis, remove in sintered specimen
Ti2Outside SbP phases, other impurity are had no.Diffraction maximum is sharp, illustrates that crystal development is good.
Specific embodiment
Form is described in further detail again to the above of the present invention by the following examples, but should not be managed this
Solve the scope for above-mentioned theme of the invention and be only limitted to below example, all technologies realized based on the above of the present invention are equal
Belong to the scope of the present invention.
Embodiment 1：
Ti powder, Sb powder, three kinds of material powders of TiP powder are Ti in molar ratio:Sb:TiP=1：1.3：1.6；Mix homogeneously, it is close
It is encapsulated in vitreosil pipe, is sintered in being put into Muffle furnace.Programming rate is 80 DEG C/min, and sintering temperature is 900 DEG C, insulation
48 hours, obtain Ti2SbP powder body materials.Ti2SbP contents are 94%.
Embodiment 2：
Ti powder, Sb powder, three kinds of material powders of TiP powder are Ti in molar ratio:Sb:TiP=1：1.2：2.0；Mix homogeneously, it is close
It is encapsulated in vitreosil pipe, is sintered in being put into Muffle furnace.Programming rate is 80 DEG C/min, and sintering temperature is 850 DEG C, insulation
24 hours, obtain Ti2SbP powder body materials.Ti2SbP contents are 88%.
Embodiment 3：
Ti powder, Sb powder, three kinds of material powders of TiP powder are Ti in molar ratio:Sb:TiP=1：0.5：2.5；Mix homogeneously, it is close
It is encapsulated in vitreosil pipe, is placed in Muffle furnace and is calcined.Programming rate is 80 DEG C/min, and sintering temperature is 850 DEG C, insulation
24 hours, obtain Ti2SbP powder body materials.Ti2SbP contents are 90%.
Embodiment 4：
Material powder is Ti in molar ratio:Sb:TiP=1：1.5：0.7；Mix homogeneously, is sealed in vitreosil pipe, puts
Calcined in Muffle furnace.Programming rate is 80 DEG C/min, and sintering temperature is 1000 DEG C, is incubated 10 hours, obtains Ti2SbP powder
Body material.Ti2SbP contents are 85%.
Embodiment 5：A kind of nothing is pressed into Ti2The method of SbP powder body materials, it comprises the steps：
1) by Ti powder, Sb powder, three kinds of raw materials of TiP powder mol ratio be Ti:Sb:TiP=1：0.8：1.2, weigh Ti powder, Sb
Powder and TiP powder raw materials, it is standby；
2) after Ti powder, Sb powder, TiP powder mix homogeneously will be weighed, it is sealed in vitreosil pipe, being placed in Muffle furnace is carried out
Calcining；
3) heating step is：1050 DEG C are risen to the heating rate of 5 DEG C/min, 36 hours are incubated；
4) after the completion of calcining, power off, natural cooling obtains Ti2SbP powder body materials.
Embodiment 6：A kind of nothing is pressed into Ti2The method of SbP powder body materials, it comprises the steps：
1) by Ti powder, Sb powder, three kinds of raw materials of TiP powder mol ratio be Ti:Sb:TiP=1：1.21：1.51, weigh Ti powder,
Sb powder, TiP powder raw materials, it is standby；
2) after Ti powder, Sb powder, TiP powder mix homogeneously will be weighed, it is sealed in vitreosil pipe, being placed in Muffle furnace is carried out
Calcining；
3) heating step is：950 DEG C are risen to the heating rate of 50 DEG C/min, 36 hours are incubated；
4) after the completion of calcining, power off, natural cooling obtains Ti2SbP powder body materials.
List of references：
[1]M.W.Barsoum.The Mn+1AXnPhases:a New Class of Solids；
Thermodynamically Stable Nanolaminates
[J].Progress in Solid State Chemistry,2000,28:201.
[2]Sundberg M,Malmqvist G,Magnusson A,EI-Raghy T.Alumina forming high
temperature silicides and carbides[J].Ceram Int,2004,30:1899.
[3]M.W.Barsoum,T.EI-Raghy.The MAX Phases:Unique New Carbide and
Nitride Materials [J].American Scientist,2001,89(4):334.
[4]“MAXTHAL Data Sheet”,3-One-2LLC,Voorhees,New Jersey.http://
www.3one2.com/
[5]“Globar Bulk Ceramic Non-inductive Resistors”,Kanthal,an affiliate
of Sandvic AB,Sandviken,Sweden.
[6]A.Yakoubi,H.Mebtouche,M.Ameri,B.Bouhafs.Structure and Bonding of
Nanolayered Ternary Phosphides[J].Materials Sciences and Applications,2011,2:
1383-1391.
[7]H.Boller.Gemischte Pnictide mit geordnetem TiP-Typ(Ti2SC-Typ)[J]
.Monatshefte fur Chemie,1973,104:166-171.
Claims (7)
1. a kind of nothing is pressed into Ti2The method of SbP powder body materials, it is characterised in that methods described comprises the steps：
1) by Ti powder, Sb powder, three kinds of raw materials of TiP powder mol ratio be Ti:Sb:TiP=1：(0.5～1.5)：(0.7～2.5),
Ti powder, Sb powder, TiP powder raw materials are weighed, it is standby；
2) after Ti powder, Sb powder, TiP mix homogeneously will be weighed, it is sealed in vitreosil pipe, is calcined in being put into Muffle furnace；
3) heating step is：800～1150 DEG C are risen to the heating rate of 5～100 DEG C/min, 10～48 hours are incubated；
4) after the completion of calcining, power off, natural cooling obtains high-purity Ti2SbP powder body materials.
2. nothing according to claim 1 is pressed into Ti2The method of SbP powder body materials, it is characterised in that：Ti powder, Sb powder, TiP
The mol ratio of three kinds of raw materials of powder is Ti:Sb:TiP=1：1.3：1.6.
3. nothing according to claim 1 is pressed into Ti2The method of SbP powder body materials, it is characterised in that：Ti powder, Sb powder, TiP
The mol ratio of three kinds of raw materials of powder is Ti:Sb:TiP=1：1.2：2.0.
4. nothing according to claim 1 is pressed into Ti2The method of SbP powder body materials, it is characterised in that：Ti powder, Sb powder, TiP
The mol ratio of three kinds of raw materials of powder is Ti:Sb:TiP=1：0.5：2.5.
5. nothing according to claim 1 is pressed into Ti2The method of SbP powder body materials, it is characterised in that：Ti powder, Sb powder, TiP
The mol ratio of three kinds of raw materials of powder is Ti:Sb:TiP=1：1.5：0.7.
6. nothing according to claim 1 is pressed into Ti2The method of SbP powder body materials, it is characterised in that：Ti powder, Sb powder, TiP
The mol ratio of three kinds of raw materials of powder is Ti:Sb:TiP=1：0.8：1.2.
7. nothing according to claim 1 is pressed into Ti2The method of SbP powder body materials, it is characterised in that：Ti powder, Sb powder, TiP
The mol ratio of three kinds of raw materials of powder is Ti:Sb:TiP=1：1.21：1.51.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102241514A (en) * | 2011-05-24 | 2011-11-16 | 武汉理工大学 | Method for synthetizing Ti3SiC2 high-purity powder |
| CN103351164A (en) * | 2013-05-23 | 2013-10-16 | 安泰科技股份有限公司 | High-purity and high-performance titanium silicon carbide ceramic block material and preparation method thereof |
| CN106032324A (en) * | 2016-04-06 | 2016-10-19 | 中国科学院金属研究所 | Method for synthesizing spherical MAX-phase powder material with main phase being Ti2AlC |
-
2016
- 2016-11-25 CN CN201611048808.2A patent/CN106518076A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102241514A (en) * | 2011-05-24 | 2011-11-16 | 武汉理工大学 | Method for synthetizing Ti3SiC2 high-purity powder |
| CN103351164A (en) * | 2013-05-23 | 2013-10-16 | 安泰科技股份有限公司 | High-purity and high-performance titanium silicon carbide ceramic block material and preparation method thereof |
| CN106032324A (en) * | 2016-04-06 | 2016-10-19 | 中国科学院金属研究所 | Method for synthesizing spherical MAX-phase powder material with main phase being Ti2AlC |
Non-Patent Citations (2)
| Title |
|---|
| （日）日本化学会编: "《无机化合物合成手册 第一卷》", 31 October 1983 * |
| Y. MEDKOUR ET AL.: ""Ab initio study of structural, electronic, and elastic properties of M2SbP (M = Ti, Zr, and Hf)"", 《EUR. PHYS. J. B》 * |
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