CN106044778A - Preparation method of high-purity tantalum disilicide powder - Google Patents
Preparation method of high-purity tantalum disilicide powder Download PDFInfo
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- CN106044778A CN106044778A CN201610534377.4A CN201610534377A CN106044778A CN 106044778 A CN106044778 A CN 106044778A CN 201610534377 A CN201610534377 A CN 201610534377A CN 106044778 A CN106044778 A CN 106044778A
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- powder
- tantalum
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- tantalum silicide
- ball milling
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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
- C01B33/00—Silicon; Compounds thereof
- C01B33/06—Metal silicides
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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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention relates to a preparation method of high-purity tantalum disilicide powder. The preparation method includes: weighing -500-mesh silicon powder, -300-mesh tantalum powder and additive NH4Cl according to the proportion, performing ball milling, evenly mixing, loading into a ceramic crucible, performing jolt ramming to achieve a certain compaction rate, loading into a combustion synthesizing furnace, vacuumizing, feeding argon, preheating, igniting to perform combustion synthesizing, cooling, and performing ball milling to obtain the needed tantalum disilicide powder. Compared with current preparation methods, the preparation method has the advantages that synthesized block mass is loose and can be broken easily, and all the block mass is tantalum-disilicide-phase tantalum disilicide powder; thereof, the single-phase tantalum disilicide powder with good granularity controllability and high purity can be prepared by the method.
Description
Technical field
The invention belongs to special powder preparing technical field, relate to a kind of side preparing tantalum silicide powder with powder for raw material
Method.
Background technology
Metal silicide have the electric conductivity of metalloid, high-temperature behavior, antioxygenic property and with silicon integrated circuit
The production technology compatibility. transition metal silicide can be used for low resistance fence gate and intraconnections, Schottky gate, Ohmic contact.Two silicon
Change tantalum there is high-melting-point, low-resistivity, anticorrosive, high temperature oxidation resistance and with the matrix material such as silicon, carbon, there is good holding concurrently
The excellent properties such as capacitive, as grid material, the link circuit of integrated circuit, high-temperature oxidation resistant coating etc., at heating, high temperature
The aspect such as structure member, electronic device has obtained wide research and application (Cui Chunjuan, Zhang Jun, Liu Lin, Fu Hengzhi, infusibility
Metal silicide TaSi2Progress, material heat treatment technology, 39 (2010) 72-74).
Tantalum silicide preparation method includes: combustion synthesis method (combustion synthesis, CS) or self propagating high temperature
Synthetic method (self-propagating high-temperature synthesis, SHS), arc melting method etc..Burning is closed
One-tenth method or self-propagating high-temperature synthesis are a kind of methods utilizing elements/compounds exothermic heat of reaction to carry out obtaining intermetallics.
It has the advantages such as equipment energy consumption simple, required is low, generated time is short, and its major defect is that response speed is fast, and process control is difficult,
Easily there is dephasign.(Yin Sheng, conbustion synthesis, Beijing: metallurgical industry publishing house, 1999).The conbustion synthesis of tantalum silicide needs
Preheating initiation reaction could realize synthesis, but there is the phase beyond disilicide.Arc melting method is it is generally required to longer homogenization
Time, the silicon loss simultaneously caused due to volatilization in fusion process may cause the generation of some dephasigns.
Plasma spray technology is up to 10000 DEG C because of its jet temperature, and effluxvelocity reaches 300-400m/s, collects high temperature melting
The advantages such as change, rapid solidification and near-net-shape are in one, and this technology is not by shape or size limitation, it is easy to accomplish its short stream
Journey preparation shapes, and is developing progressively as a kind of novel parts forming technique, is already used to prepare some parts.Utilize
Tantalum silicide powder is made bulk by plasma spraying technology preparation, and (Zhu Yaran, general intelligent, Huang Lisheng, one prepares tantalum silicide block
The method of body material, ZL201410125984.6), this needs high-purity tantalum silicide powder as raw material.Therefore, how to obtain
High-purity tantalum silicide (not having dephasign to generate) powder becomes crucial.
Summary of the invention
For overcoming the existing deficiency preparing tantalum silicide powder, the present invention provides a kind of and novel prepares tantalum silicide powder
The method at end.
The technical scheme is that the preparation method that a kind of high-purity tantalum silicide powder is provided, it is characterised in that include as
Lower step:
1)-500 mesh silica flours and-300 mesh tantalum powder are pressed TaSi2Stoichiometric proportion weigh；
2) addition accounts for silica flour and the NH of tantalum grain weight amount 0.5-1.5%4Cl powder；
3) by above-mentioned powder ball milling, ratio of grinding media to material 4:1-8:1, Ball-milling Time 8-12 hour；
Being loaded in silicon carbide crucible by powder after ball milling, putting jolt ramming on a vibration table to relative density is 35-40%；
4) crucible of dress powder is loaded in synthetic furnace, be filled with argon after evacuation, be warming up to 450-with 15-20 DEG C per minute
650 DEG C, ignite tantalum silicide synthetic reaction with tungsten filament energising；
5) obtain final powder-product with zirconia ball and tank are broken after cooling, detect all tantalum silicide phases through XRD.
Compared with existing manufacture method, the synthesis agglomerate of the inventive method is loose, is easily broken, and all tantalum silicides
The tantalum silicide powder of phase.Therefore, the inventive method can prepare that to have granularity controllability good, the single-phase tantalum silicide that purity is high
Powder.
Accompanying drawing explanation
Fig. 1 is Si-Ta binary phase diagraml；
Fig. 2 is TaSi prepared by the present invention2The XRD figure of powder.
Detailed description of the invention
In combustion synthesis technology, TaSi2Synthesis mixed with silica flour by tantalum powder and be heated under uniform temperature, igniting is drawn
Send out what the exothermic reaction between tantalum and Si powder completed.Owing to this system is weak heat release system, so to heat in advance, make heat release
Reaction can self-sustaining.Owing to Ta-Si system there is also other compound, as it is shown in figure 1, include Ta5Si3、Ta2Si、
Ta3Si, therefore at synthesis TaSi2Time, as improper in controlled, it is easy to obtain other tantalum silicide phase.
In the methods of the invention, the TaSi of the present invention2Powder preparation method comprises the steps:
First ,-500 mesh silica flours and-300 mesh tantalum powder are pressed TaSi2Stoichiometric proportion weigh.Highly purified herein for obtaining
Product, needs to select highly purified silica flour and tantalum powder, such as purity 99.95 or 99.99%.Select-500 mesh silica flours and-300 mesh
It is to preferably make silicon mix homogeneously with tantalum that tantalum powder coordinates, and makes tantalum particle be surrounded by silicon grain, and be conducive to burning below conjunction
The step become makes to be easier between silicon and tantalum haptoreaction.Using stoichiometric is to obtain TaSi2Phase.All make
In the case of-200 mesh or-300 mesh silica flours and tantalum powder, it is difficult to obtain the most single-phase TaSi2Phase powder, the most a small amount of
Ta5Si3Phase.The material powder using granularity less can make reaction more complete, but this increases oxygen content in power, can hinder on the contrary
Hinder synthetic reaction.
Second, add silica flour and the NH of tantalum grain weight amount 0.5-1.5%4Cl powder.Research finds NH4Cl is to silicon and the reaction of tantalum
Play catalytic action, it is possible to accelerate reaction therebetween and make reaction carry out the most completely.When there is no ammonium chloride, the most instead
Should be incomplete, other tantalum silicide phase can be remained.
3rd, by above-mentioned powder ball milling, ratio of grinding media to material 4:1-8:1, Ball-milling Time 8-12 hour.Under this ball milling parameter, former
Material mix homogeneously, contact fully, is reacted more complete.
4th, the powder after ball milling is loaded in silicon carbide crucible, putting jolt ramming on a vibration table to relative density is 35-
40%.Using silicon carbide crucible heat conduction good, heat-resisting, reaction Fast exothermic will not make crucible damage.Jolt ramming is to relative density 35-
40%, on the one hand granule contact is fully, on the other hand keeps relative loose, is easily broken after reaction, it is easy to controls product granularity
Size.
5th, the crucible of dress powder is loaded in synthetic furnace, is filled with argon after evacuation, with 15-20 DEG C of intensification per minute
To 450-650 DEG C, ignite tantalum silicide synthetic reaction with tungsten filament energising.Evacuation is filled with argon, anti-oxidation.Be rapidly heated speed
Degree is to prevent pilot process from generating other tantalum silicide.High preheating temperature is able to ensure that lights reactive combustion synthesis all lifes
Become TaSi2Phase.
6th, obtain final powder-product with zirconia ball and tank are broken after cooling, detect all tantalum silicides through XRD
Phase.Impurity can be reduced with zirconium oxide ball milling to introduce, particularly prevent the introducing of ferrum.Under the comprehensive function of above measure, this
Inventive method can control silica flour and the reaction of tantalum powder, as in figure 2 it is shown, all generate TaSi through XRD detection2Phase.
Below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment 1
-500 mesh silica flour 23.6 grams and 76.4 grams of-300 mesh tantalum powder are weighed；
Add and account for silica flour and the NH of tantalum grain weight amount 0.5 gram4Cl powder；
By above-mentioned powder ball milling, ratio of grinding media to material 8:1, Ball-milling Time 12 hours；
Being loaded in silicon carbide crucible by powder after ball milling, putting jolt ramming on a vibration table to relative density is 40%；
The crucible of dress powder is loaded in synthetic furnace, is filled with argon after evacuation, is warming up to 650 DEG C with 20 DEG C per minute, uses tungsten
Silk energising is ignited tantalum silicide synthetic reaction；
Obtain final powder-product with zirconia ball and tank are broken after cooling, detect all tantalum silicide phases through XRD.
Embodiment 2
-500 mesh silica flour 23.6 grams and 76.4 grams of-300 mesh tantalum powder are weighed；
Add and account for silica flour and the NH of tantalum grain weight amount 1.5 grams4Cl powder；
By above-mentioned powder ball milling, ratio of grinding media to material 4:1, Ball-milling Time 8 hours；
Being loaded in silicon carbide crucible by powder after ball milling, putting jolt ramming on a vibration table to relative density is 35%；
The crucible of dress powder is loaded in synthetic furnace, is filled with argon after evacuation, is warming up to 450 DEG C with 15 DEG C per minute, uses tungsten
Silk energising is ignited tantalum silicide synthetic reaction；
Obtain final powder-product with zirconia ball and tank are broken after cooling, detect all tantalum silicide phases through XRD.
Embodiment 3
-500 mesh silica flour 23.6 grams and 76.4 grams of-300 mesh tantalum powder are weighed；
Add and account for silica flour and the NH of tantalum grain weight amount 1.0 grams4Cl powder；
By above-mentioned powder ball milling, ratio of grinding media to material 6:1, Ball-milling Time 10 hours；
Being loaded in silicon carbide crucible by powder after ball milling, putting jolt ramming on a vibration table to relative density is 38%；
The crucible of dress powder is loaded in synthetic furnace, is filled with argon after evacuation, is warming up to 550 DEG C with 18 DEG C per minute, uses tungsten
Silk energising is ignited tantalum silicide synthetic reaction；
Obtain final powder-product with zirconia ball and tank are broken after cooling, detect all tantalum silicide phases through XRD.
Embodiment 4
-500 mesh silica flour 23.6 grams and 76.4 grams of-300 mesh tantalum powder are weighed；
Add and account for silica flour and the NH of tantalum grain weight amount 0.8 gram4Cl powder；
By above-mentioned powder ball milling, ratio of grinding media to material 7:1, Ball-milling Time 11 hours；
Being loaded in silicon carbide crucible by powder after ball milling, putting jolt ramming on a vibration table to relative density is 39%；
The crucible of dress powder is loaded in synthetic furnace, is filled with argon after evacuation, is warming up to 600 DEG C with 19 DEG C per minute, uses tungsten
Silk energising is ignited tantalum silicide synthetic reaction；
Obtain final powder-product with zirconia ball and tank are broken after cooling, detect all tantalum silicide phases through XRD.
Embodiment 5
-500 mesh silica flour 23.6 grams and 76.4 grams of-300 mesh tantalum powder are weighed；
Add and account for silica flour and the NH of tantalum grain weight amount 1.2 grams4Cl powder；
By above-mentioned powder ball milling, ratio of grinding media to material 5:1, Ball-milling Time 9 hours；
Being loaded in silicon carbide crucible by powder after ball milling, putting jolt ramming on a vibration table to relative density is 36%；
The crucible of dress powder is loaded in synthetic furnace, is filled with argon after evacuation, is warming up to 500 DEG C with 16 DEG C per minute, uses tungsten
Silk energising is ignited tantalum silicide synthetic reaction；
Obtain final powder-product with zirconia ball and tank are broken after cooling, detect all tantalum silicide phases through XRD.
Therefore, the inventive method by integrating raw material granularity, additive, ball milling, load and the synthesis that heats up etc. is all multi-ring
Joint, makes course of reaction easily controllable, it is possible to obtain simple TaSi2The dusty material of phase, and by control material purity with
And avoid process to introduce impurity, thus finally obtain highly purified single-phase TaSi2Powder.
Claims (4)
1. a high-purity tantalum silicide powder preparation method, it is characterised in that comprise the steps:
1)-500 mesh silica flours and-300 mesh tantalum powder are pressed TaSi2Stoichiometric proportion weigh；
2) NH is added4Cl powder；
3) by above-mentioned powder ball milling, ratio of grinding media to material 4:1-8:1, Ball-milling Time 8-12 hour；
4) powder after ball milling is loaded in silicon carbide crucible, put jolt ramming on a vibration table；
5) crucible of dress powder is loaded in synthetic furnace, after evacuation, be filled with argon, heat up, ignite with tungsten filament energising tantalum silicide
Synthetic reaction；
6) obtain final powder-product with zirconia ball and tank are broken after cooling, detect all tantalum silicide phases through XRD.
A kind of high-purity tantalum silicide powder preparation method the most as claimed in claim 1, it is characterised in that step 2) step 2) described
NH4Cl powder accounts for silica flour and tantalum grain weight amount 0.5-1.5%.
A kind of high-purity tantalum silicide powder preparation method the most as claimed in claim 1, it is characterised in that jolt ramming phase described in step 4)
It is 35-40% to density.
A kind of high-purity tantalum silicide powder preparation method the most as claimed in claim 1, it is characterised in that heat up described in step 5) speed
Rate is 15-20 DEG C per minute, warming temperature 450-650 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610534377.4A CN106044778A (en) | 2016-07-07 | 2016-07-07 | Preparation method of high-purity tantalum disilicide powder |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610534377.4A CN106044778A (en) | 2016-07-07 | 2016-07-07 | Preparation method of high-purity tantalum disilicide powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408394A (en) * | 2020-11-23 | 2021-02-26 | 武汉科技大学 | Preparation method of tantalum disilicide nano powder |
| CN114538450A (en) * | 2020-11-27 | 2022-05-27 | 有研工程技术研究院有限公司 | High-purity tantalum disilicide powder and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100043877A1 (en) * | 2008-08-25 | 2010-02-25 | The Trustees Of Boston College | Hetero-Nanostructures for Solar Energy Conversions and Methods of Fabricating Same |
| CN103882368A (en) * | 2014-03-31 | 2014-06-25 | 中国科学院上海硅酸盐研究所 | Method for preparing tantalum disilicide coating |
-
2016
- 2016-07-07 CN CN201610534377.4A patent/CN106044778A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100043877A1 (en) * | 2008-08-25 | 2010-02-25 | The Trustees Of Boston College | Hetero-Nanostructures for Solar Energy Conversions and Methods of Fabricating Same |
| CN103882368A (en) * | 2014-03-31 | 2014-06-25 | 中国科学院上海硅酸盐研究所 | Method for preparing tantalum disilicide coating |
Non-Patent Citations (2)
| Title |
|---|
| C.L.YEH ET AL: "A comparative study on combustion synthesis of Ta-Si compounds", 《INTERMETALLICS》 * |
| 张红波 等: "自蔓延制备高纯二硅化钼粉体", 《稀有金属材料与工程》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408394A (en) * | 2020-11-23 | 2021-02-26 | 武汉科技大学 | Preparation method of tantalum disilicide nano powder |
| CN112408394B (en) * | 2020-11-23 | 2023-07-07 | 武汉科技大学 | Preparation method of tantalum disilicide nano powder |
| CN114538450A (en) * | 2020-11-27 | 2022-05-27 | 有研工程技术研究院有限公司 | High-purity tantalum disilicide powder and preparation method thereof |
| CN114538450B (en) * | 2020-11-27 | 2023-08-15 | 有研工程技术研究院有限公司 | High-purity tantalum disilicide powder and preparation method thereof |
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