CN205419809U - A device for preparing chemical vapor deposition metal precursor for rhenium - Google Patents
A device for preparing chemical vapor deposition metal precursor for rhenium Download PDFInfo
- Publication number
- CN205419809U CN205419809U CN201520840981.0U CN201520840981U CN205419809U CN 205419809 U CN205419809 U CN 205419809U CN 201520840981 U CN201520840981 U CN 201520840981U CN 205419809 U CN205419809 U CN 205419809U
- Authority
- CN
- China
- Prior art keywords
- catcher
- collector
- oxygen
- rhenium
- tube
- 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.)
- Withdrawn - After Issue
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- 239000002184 metal Substances 0.000 title claims abstract description 22
- 229910052702 rhenium Inorganic materials 0.000 title claims abstract description 21
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 20
- 238000005229 chemical vapour deposition Methods 0.000 title abstract description 4
- 239000002243 precursor Substances 0.000 title abstract description 3
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052756 noble gas Inorganic materials 0.000 claims description 13
- 239000011324 bead Substances 0.000 claims description 10
- 239000007792 gaseous phase Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 238000000151 deposition Methods 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 8
- 238000000034 method Methods 0.000 abstract description 13
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 239000011261 inert gas Substances 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 description 23
- 229910002785 ReO3 Inorganic materials 0.000 description 7
- XZQYTGKSBZGQMO-UHFFFAOYSA-I Rhenium(V) chloride Inorganic materials Cl[Re](Cl)(Cl)(Cl)Cl XZQYTGKSBZGQMO-UHFFFAOYSA-I 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 5
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- 229910001882 dioxygen Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910021634 Rhenium(III) chloride Inorganic materials 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- YEWLVPDHCCERJH-UHFFFAOYSA-N [Re].[Ir] Chemical compound [Re].[Ir] YEWLVPDHCCERJH-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- LOIHSHVELSAXQN-UHFFFAOYSA-K trirhenium nonachloride Chemical compound Cl[Re](Cl)Cl LOIHSHVELSAXQN-UHFFFAOYSA-K 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The utility model discloses a device for preparing chemical vapor deposition metal precursor for rhenium belongs to the NULL field, the utility model provides a device including inert gas collector, oxygen collector, psammitolite filter ball, tube -like stove, collector I, collector II, rectification pipe, add the heating bath pot, the inert gas collector, the oxygen collector is equal and psammitolite filter ball's one end intercommunication, psammitolite filter ball lies in the tube -like stove, psammitolite filter ball's the other end and collector I feed through, collector I lies in with the heating bath pot, collector I and rectification pipe intercommunication, and the bottom and the collector II of rectification pipe feed through, device reaction efficiency is high, and reOCl4 and reO3Cl separate through the method of rectification very much, have improved result reOCl4's purity.
Description
Technical field
This utility model discloses a kind of device for preparing chemical gaseous phase deposition rhenium metal presoma, belongs to technical field of material, is applied to aviation rhenium iridium nozzle.
Background technology
Rhenium metal fusing point is high, there is the characteristics such as the high-temperature mechanics of excellence, thermal fatigue resistance, wear-resisting, anticorrosive and catalysis, it is widely used in national defence, Aero-Space, electronics and field of petrochemical industry, such as: thermionic emission material, high-temperature engine thrust chamber jet pipe etc..But owing to rhenium metal fusing point is higher, general employing powder metallurgic method processing；For aerial metal rhenium pipe, owing to working condition is severe, the material internal defect using powder metallurgic method to prepare is more, the most easily generates cracking failure, and the effective time reduces.Chemical gaseous phase deposition is a kind of newly net forming technique preparing high temperature difficult-to-machine metal that development in recent years is got up, and resulting product purity is higher, and density is close to theoretical value.The advanced technology countries such as the U.S. use chemical vapour deposition technique to be successfully prepared the rhenium metal pipe of function admirable, have been successfully applied to the high temperature jet pipe of rocket, satellite and guided missile.
The document of the openest report is pointed out, typically uses ReCl5As presoma, although compound R eCl5Boiling point is 300 DEG C, but it i.e. starts to decompose at 180 DEG C, obtains another compound R eCl of rhenium metal3.Even if temperature is raised to 600 DEG C of beginning chemical gaseous phase depositions, compound R eCl5Decompose in addition to obtaining rhenium metal, still have product ReCl3.Compound R eCl3When about 400 DEG C, it is likely to be obtained again compound R eCl5, when only reaching more than 1000 DEG C, compound R eCl3It is only possible to be decomposed into rhenium metal, and compound R eCl3Can be stable in the presence of 2000 DEG C and more than.Thus in whole chemical vapor deposition method, the control of parameter must take into account the decomposition of two kinds of compounds, easily affect organizational structure and the performance of rhenium metal, and the sedimentation rate of rhenium metal and the utilization rate of raw material.
And ReOCl4, boiling point is at 220 DEG C, and its gas phase can be stabilized to 700 DEG C always and not decompose.Rhenium metal and compound R eO is started to decompose into more than 700 DEG C3Cl, versus compound ReCl5For, compound R eOCl4Presoma as chemical gaseous phase deposition has the advantage that (1) process parameter control is simple, because of compound R eO3Even if Cl also will not decompose more than 2000 DEG C；(2) raw material availability is high, can be to more than 60%, close to theoretical utilization rate 66%；(3) sedimentation rate is fast, is to use compound R eCl510 times.Consider from the feature of this performance and its saturated vapor pressure, compound R eOCl4It it is alternative compounds ReCl5Ideal substitute as rhenium metal vapor deposition precursor body.
Preparation method ReOCl at present4Preparation method more.Wherein, a kind of preferable preparation method is that the sulfuryl chloride by excess acts on rhenium metal when 300 DEG C, but the method preparation temperature is higher and at high temperature sulfuryl chloride easily decomposes, so preparation efficiency is relatively low.Additionally can be with ReO3With ReCl5, reaction prepare ReOCl4.But use said method to prepare ReOCl before using4Time, ReOCl4Meeting and ReO3Reaction generates ReCl3And ReO3Cl, makes productivity reduce.
Summary of the invention
The purpose of this utility model is to provide a kind of device for preparing chemical gaseous phase deposition rhenium metal presoma, equipment therefor includes noble gas catcher 1, oxygen catcher 2, core filter bulb 3, tube furnace 4, catcher I 5, catcher II 6, bead tube 7, adds heat bath pan 8, noble gas catcher 1, oxygen catcher 2 all connect with one end of core filter bulb 3, core filter bulb 3 is positioned at tube furnace 4, and the other end of core filter bulb 3 connects with catcher I 5；Catcher I 5 is positioned at and adds heat bath pan 8, and catcher I 5 connects with bead tube 7, and the bottom of bead tube 7 connects with catcher II 6.
Preferably, noble gas catcher 1 exit described in the utility model is provided with valve I 9, oxygen catcher 2, valve II 10.
Use process of the present utility model is: by ReCl5It is placed in the core surface of core filter bulb, and core filter bulb is placed in tube furnace is heated to reaction temperature, make ReCl by adjusting high purity inert gas and high purity oxygen gas pressure, flow5Fully react with oxygen, and utilize core that reactant, product are carried out effective solid-liquid-gas separation, simultaneously by product ReOCl4And ReO3Cl concentrates in the collection container of oil bath pan heating, after question response, closes oxygen, keeps noble gas circulation, and is lowered the temperature by tube furnace, and heating oil bath pan makes ReO simultaneously3Cl is volatized into rectification cell and collects, and purifies ReOCl4, it is thus achieved that chemical gaseous phase deposits the high-purity presoma ReOCl of rhenium metal4。
The beneficial effects of the utility model: this utility model uses core filter bulb device, build solid-liquid-gas piece-rate system, by solid compounds ReCl5With product ReOCl4And ReO3Cl, and product gas Cl2, reactor off-gas carry out high efficiency separation；On the one hand reactant contact area is big, and reaction efficiency is high, and productivity is high；Simultaneously by distillation system, by product ReOCl4And ReO3Cl separates, and improves product ReOCl4Purity；Owing to whole system is closed gas circuit, process parameter control is easy, and reaction rate is fast, and productivity is high, and free from admixture pollutes, and product purity is high.
Accompanying drawing explanation
Fig. 1 is the structural representation of this utility model equipment therefor.
In figure: 1-noble gas catcher；2-oxygen catcher；3-core filter bulb；4-tube furnace；5-catcher I；6-catcher II；7-bead tube；8-adds heat bath pan；9-valve I；10-valve II；11-valve III.
Detailed description of the invention
With specific embodiment, this utility model is described in further detail below in conjunction with the accompanying drawings, but protection domain of the present utility model is not limited to described content.
Embodiment 1:
For preparing the device of chemical gaseous phase deposition rhenium metal presoma described in the present embodiment, as shown in Figure 1, including noble gas catcher 1, oxygen catcher 2, core filter bulb 3, tube furnace 4, catcher I 5, catcher II 6, bead tube 7, add heat bath pan 8, noble gas catcher 1, oxygen catcher 2 all connect with one end of core filter bulb 3, core filter bulb 3 is positioned at tube furnace 4, and the other end of core filter bulb 3 connects with catcher I 5；Catcher I 5 is positioned at and adds heat bath pan 8, and catcher I 5 connects with bead tube 7, and the bottom of bead tube 7 connects with catcher II 6；Noble gas catcher 1 exit is provided with valve I 9, oxygen catcher 2, valve II 10.
The use process of device described in the present embodiment is:
(1) powder ReCl is weighed5It is placed in core filter bulb, uniformly paves；Being placed in tube furnace by core filter bulb, connected by whole system pipeline sealing, ground connection is all fixed with rustless steel chuck, checks air-tightness；Start valve and be passed through nitrogen, be carried out technique, nitrogen pressure: 0.1MPa, flow: 0.1L/ minute, clean whole pipeline 50 minutes；Starting valve and be passed through high purity oxygen gas (>=99.9%), oxygen pressure: 0.1MPa, flow: 0.05L/ minute, noble gas controls as 2:1, stably supply 2 minutes with oxygen flow ratio；Start tube furnace, be incubated from room temperature to 120 DEG C with 1 DEG C/min programming rate.
(3) oil bath pan temperature controls at 20 DEG C, compound R eOCl4With compound R eO3Cl is present in collection container bottom in liquid form；Until not producing yellow green gas Cl2, reaction terminates；Closing high purity oxygen gas valve, continue to be passed through noble gas 20 minutes, tube furnace is cooled to 90 DEG C of insulations；Oil bath pan temperature is increased to 130 DEG C, makes compound R eO3Cl is volatized into distillation system and is condensed into colorless liquid, is dark brown ReOCl bottom catcher I 54；Under keeping nitrogen circulation situation, whole system is cooled to room temperature, collects compound R eOCl respectively4And compound R eO3Cl, respectively obtains 61 grams of solid compounds ReOCl4, and 22 grams of liquefied compound ReO3Cl, ReOCl4Productivity is 96%.
Claims (2)
1. the device depositing rhenium metal presoma for preparing chemical gaseous phase, it is characterized in that: include noble gas catcher (1), oxygen catcher (2), core filter bulb (3), tube furnace (4), catcher I (5), catcher II (6), bead tube (7), add heat bath pan (8), noble gas catcher (1), oxygen catcher (2) all one end with core filter bulb (3) connect, core filter bulb (3) is positioned at tube furnace (4), and the other end of core filter bulb (3) connects with catcher I (5)；Catcher I (5) is positioned at and adds heat bath pan (8), and catcher I (5) connects with bead tube (7), and the bottom of bead tube (7) connects with catcher II (6).
The most according to claim 1 for preparing the device of chemical gaseous phase deposition rhenium metal presoma, it is characterised in that: noble gas catcher (1) exit is provided with valve I (9), oxygen catcher (2), valve II (10).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520840981.0U CN205419809U (en) | 2015-10-28 | 2015-10-28 | A device for preparing chemical vapor deposition metal precursor for rhenium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520840981.0U CN205419809U (en) | 2015-10-28 | 2015-10-28 | A device for preparing chemical vapor deposition metal precursor for rhenium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN205419809U true CN205419809U (en) | 2016-08-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201520840981.0U Withdrawn - After Issue CN205419809U (en) | 2015-10-28 | 2015-10-28 | A device for preparing chemical vapor deposition metal precursor for rhenium |
Country Status (1)
| Country | Link |
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| CN (1) | CN205419809U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105253917A (en) * | 2015-10-28 | 2016-01-20 | 昆明理工大学 | Method for preparing precursor for chemical vapor deposition of metallic rhenium |
-
2015
- 2015-10-28 CN CN201520840981.0U patent/CN205419809U/en not_active Withdrawn - After Issue
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105253917A (en) * | 2015-10-28 | 2016-01-20 | 昆明理工大学 | Method for preparing precursor for chemical vapor deposition of metallic rhenium |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned | ||
| AV01 | Patent right actively abandoned | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20160803 Effective date of abandoning: 20170728 |
|
| AV01 | Patent right actively abandoned |
Granted publication date: 20160803 Effective date of abandoning: 20170728 |