CN103727317A - Manufacturing method of rhenium-based refractory metal hybrid tube - Google Patents

Manufacturing method of rhenium-based refractory metal hybrid tube Download PDF

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CN103727317A
CN103727317A CN201310410630.1A CN201310410630A CN103727317A CN 103727317 A CN103727317 A CN 103727317A CN 201310410630 A CN201310410630 A CN 201310410630A CN 103727317 A CN103727317 A CN 103727317A
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rhenium
tube
foam
layer
cvd
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CN103727317B (en
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陈照峰
聂丽丽
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Taicang Paiou Technology Consulting Service Co Ltd
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Taicang Paiou Technology Consulting Service Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/028—Including graded layers in composition or in physical properties, e.g. density, porosity, grain size

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemically Coating (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

Disclosed is a manufacturing method of a rhenium-based refractory metal hybrid tube. The tube comprises a nickel coating, a rhenium foam layer, a metal rhenium layer and an iridium coating. The method is characterized by comprising the steps of (1) conducing pyrolysis on a polyurethane foam tube with a certain thickness to obtain a carbon foam tube, (2) depositing a rhenium film on the wall of a carbon foam hole with the CVD method with ReC15 as the precursor to obtain a rhenium foam tube, (3) preparing the rhenium metal layer on the inner surface of rhenium foam with the CVD method with the ReC15 as the precursor, (4) preparing the iridium coating with a certain thickness on the surface of the rhenium metal layer with the CVD/DGP method, and (5) preparing a nickel-plated layer with a certain thickness on the outmost layer of the tube, namely on the outer surface of the rhenium foam tube with the electroforming method. Atomic force combination exists between layers of the hybrid material manufactured with the method, the weight is low, strength is high, high-temperature performance is excellent, and oxidation resistance and corrosion resistance are achieved. The rhenium-based refractory metal hybrid tube manufactured with the method can serve as a high-demanding aerospace vehicle spray tube and other high-temperature structural members.

Description

A kind of rhenium base refractory metal mixes the preparation method of pipe
Technical field
The present invention relates to a kind of preparation method of tubular material, particularly relate to the preparation method that a kind of rhenium base refractory metal mixes pipe.
Background technique
As the pure refractory metal of one, rhenium is attractive especially for the thermal structure such as space flight and missile propulsion system and energy source device.The lining combining as structural material or with graphite, carbon/carbon structure material, rhenium can meet the requirement against corrosion of high temperature rocket motor and hot gas valve part.Compared with some other alternative lining material, rhenium has many advantages.Its fusing point is 3180 ℃, has exceeded other metal except tungsten, still, different from tungsten, and the brittle-ductile transition temperature of rhenium is widely lower than room temperature.When temperature is brought up to 2700 ℃ from room temperature, the extension plasticity of rhenium is about 35%, and tensile strength drops to 48MPa left and right from about 1127MPa.Rhenium is actually very blunt to thermal shock.In addition, the propulsion device jet pipe being processed by rhenium has withstood from the thermal fatigue loop around test of more than 100,000 time more than room temperature to 2200 ℃ and without any the sign destroying.As the coating on material with carbon element, rhenium is unique a kind of refractory metal that does not form carbide.And rhenium is very large to the solubility of carbon, can guarantee to obtain between bi-material very high join strength.Through repeatedly studies have shown that, the performance of rhenium is all better than whole other coatings on the part of solid propellant rocket hot-zone.
Publication number be the Chinese invention patent of 101899693A a kind of electroplate liquid formulation that plates rhenium on oxygen-free copper matrix and compound method are disclosed and on oxygen-free copper matrix the method for locally plating rhenium, electroplate liquid formulation is rehenic acid potassium 15～20g/l; Nickelous sulfate 4～6g/l; Ammonium sulfate 50～60g/l, the method for plating rhenium comprises pickling, plating rhenium, on oxygen-free copper matrix, needs the surface of rhenium layer to coat perchloro-ethylene lacquer, hydrogen peroxide except rhenium.The present invention is plated rhenium solution formula, is optimized plating rhenium technique by improvement, improves the method for locally plating rhenium, makes the rhenium layer even compact of plating, and adhesion is good, not volatile feature after hydrogen stove high-temperature heat treatment.
Publication number is that the Chinese invention patent of 102430431A discloses a kind of highly active supported organic rhenium catalyst take basic zirconium phosphate class stratified material as carrier belonging to catalyst preparation technical field and preparation method thereof.It is carrier that the present invention selects the Zirconium phosphate compound with stratiform structure, the methyl rhenium trioxide with catalytic activity is anchored on to the surface of Zirconium phosphate compound, thereby has obtained supported organic rhenium catalyst.This catalyzer is applied to catalyzing expoxidation of olefines synthesizing epoxy compound, and reaction-ure conversion-age is high, and the selectivity of product is high.
Summary of the invention
The present invention, mainly for the thermal structure pipe fitting of burner, proposes the preparation method that a kind of rhenium base refractory metal mixes pipe.This tubing is comprised of four layers of different materials, is nickel coating, rhenium foam layer, rhenium metal layer and iridium coating layer from outside to inside successively, and thickness is respectively 0.5～3mm, 1～5mm, 0.1～0.5cm and 0.1mm～0.5mm.By active force between atom, combine between layers, can be at stable operation under hot environment, and anti-oxidant, corrosion protection, can be used as high temperature structural members such as requiring harsh aerospace vehicle jet pipe.
Rhenium base refractory metal mixes a preparation method for pipe, it is characterized in that comprising the step of following order:
(1) pyrolysis of certain thickness polyurethane foam pipe is made to carbon foam tube;
(2) with ReCl 5for precursor, by the method for CVD, in carbon foam cell walls, deposit rhenium film, obtain rhenium foam tube;
(3) with ReCl 5for precursor, by the method for CVD, in rhenium foam interior surface, prepare rhenium metal layer;
(4) adopt the method for CVD to prepare certain thickness iridium coating layer at rhenium layer on surface of metal;
(5) adopt the method for electroforming at the outermost surface of tubing, the outer surface of rhenium foam tube is prepared certain thickness nickeling layer.
According to above-mentioned preparation method, the concrete manufacturing process of described carbon foam tube is: first in air, polyurethane foam pipe is heated at 200～255 ℃; Then make body material carbonization in inert atmosphere, at 700～900 ℃, obtain carbon foam tube.
Described CVD method deposition rhenium film and the manufacturing process of rhenium metal layer are: will after carbon foam tube outer surface graphite paper parcel, put into CVD stove, temperature setting is set to 900～1200 ℃, ReCl 5molecular Adsorption is at carbon foam tube internal surface and decomposite rhenium atom, and rhenium atom is attached to carbon foam hole inwall equably, finally forms a kind of internal surface and be covered with the rhenium foam tube of rhenium metal layer.
The concrete preparation process of described CVD iridium coating layer is: take praseodynium iridium as pioneer, at 180～250 ℃, make its volatilization, deposition occurs to decompose in the substrate that is heated to 500～600 ℃.
The actual conditions of described electroformed nickel coating is: take nickelous sulfate as main salt, and 40～60 ℃ of temperature, direct current supply, current density is 1.0～3.0A/dm 2.
Major advantage of the present invention is: the hybrid materials that 1. prepared by the method have atomic force combination between layers, and quality is light, and intensity is high, have excellent high-temperature behavior, can anti-oxidant and corrosion protection; 2. mainly adopt chemical meteorology deposition method and electroplating technology, technology maturation, simple to operate, efficiency is high, and coating quality is stable; 3. at material surface, be prepared with anti-oxidant, corrosion resistant coating, dependency structure part has long service life, the advantage of good stability.
Accompanying drawing explanation
Be illustrated as the schematic diagram that a kind of rhenium base refractory metal mixes pipe.
Diagram 10 is nickel coating; 20 is rhenium foam; 30 is rhenium metal tube; 40 is iridium coating layer.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiments is only not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims to the modification of the various equivalent form of values of the present invention and limit.
Embodiment 1
Rhenium base refractory metal mixes a preparation method for pipe, comprises the step of following order:
(1) preparing aperture is 5mm, the polyurethane foam pipe that wall thickness is 0.2cm;
(2) by the polyurethane foam pipe that makes first in air, heating at 200 ℃, then in nitrogen atmosphere, carbonization at 900 ℃, obtain carbon foam tube;
(3) carbon foam tube outer surface is put into CVD stove with after graphite paper parcel, temperature is heated to 1050 ℃, ReCl 5molecular Adsorption is at carbon foam tube internal surface and decomposite rhenium atom, and rhenium atom is attached to carbon foam hole inwall equably, finally forms a kind of internal surface and be covered with the rhenium foam tube of rhenium metal layer;
(4) take praseodynium iridium as pioneer, at 230 ℃, make its volatilization, pass in CVD stove, pioneer occurs to decompose deposition at the internal surface of pipe that is heated to 600 ℃, in the control time, obtains certain thickness iridium coating layer;
(5) internal surface of aforementioned tubes and side are pasted with insulating tape, put into the electronickelling solution preparing, connect D.C. regulated power supply, control electric current and time, at pipe outer surface, plate certain thickness nickel coating.
The tubular material of the specific admixture that said method makes, this material is comprised of four layers of different materials, nickel coating, rhenium foam layer, rhenium metal layer and iridium coating layer from outside to inside successively, the thickness that wherein wall thickness of rhenium foam tube is original polyurethane tube, be 5mm, the thickness of other layer is controlled according to concrete preparation technology parameter.
Embodiment 2
Rhenium base refractory metal mixes a preparation method for pipe, comprises the step of following order:
(1) preparing aperture is 4mm, the polyurethane foam pipe that wall thickness is 0.5cm;
(2) by the polyurethane foam pipe that makes first in air, heating at 250 ℃, then in nitrogen atmosphere, carbonization at 850 ℃, obtain carbon foam tube;
(3) carbon foam tube outer surface is put into CVD stove with after graphite paper parcel, temperature is heated to 1150 ℃, ReCl 5molecular Adsorption is at carbon foam tube internal surface and decomposite rhenium atom, and rhenium atom is attached to carbon foam hole inwall equably, finally forms a kind of internal surface and be covered with the rhenium foam tube of rhenium metal layer;
(4) take praseodynium iridium as pioneer, at 220 ℃, make its volatilization, pass in CVD stove, pioneer occurs to decompose deposition at the internal surface of pipe that is heated to 600 ℃, in the control time, obtains certain thickness iridium coating layer;
(5) internal surface of aforementioned tubes and side are pasted with insulating tape, put into the electronickelling solution preparing, connect D.C. regulated power supply, control electric current and time, at pipe outer surface, plate certain thickness nickel coating.
The tubular material of the specific admixture that said method makes, this material is comprised of four layers of different materials, nickel coating, rhenium foam layer, rhenium metal layer and iridium coating layer from outside to inside successively, the thickness that wherein wall thickness of rhenium foam tube is original polyurethane tube, be 3mm, the thickness of other layer is controlled according to concrete preparation technology parameter.
Above are only two embodiments of the present invention, but design concept of the present invention is not limited to this, allly utilizes this design to carry out the change of unsubstantiality to the present invention, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content that does not depart from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.

Claims (5)

1. rhenium base refractory metal mixes a preparation method for pipe, comprises nickel coating, rhenium foam layer, rhenium metal layer and iridium coating layer, it is characterized in that comprising the step of following order:
(1) pyrolysis of certain thickness polyurethane foam pipe is made to carbon foam tube;
(2) with ReCl 5for precursor, by the method for CVD, in carbon foam cell walls, deposit rhenium film, obtain rhenium foam tube;
(3) with ReCl 5for precursor, by the method for CVD, in rhenium foam interior surface, prepare rhenium metal layer;
(4) adopt the method for CVD to prepare certain thickness iridium coating layer at rhenium layer on surface of metal;
(5) adopt the method for electroforming at the outermost surface of tubing, the outer surface of rhenium foam tube is prepared certain thickness nickeling layer.
2. preparation method according to claim 1, is characterized in that described carbon foam tube obtains by the pyrolysis of polyurethane foam pipe, and concrete manufacturing process is: first in air, polyurethane foam pipe is heated at 200～255 ℃; Then make body material carbonization in inert atmosphere, at 700～900 ℃.
3. preparation method according to claim 1, is characterized in that described CVD method deposition rhenium film and the manufacturing process of rhenium metal layer are: will after carbon foam tube outer surface graphite paper parcel, put into CVD stove, temperature setting is set to 900～1200 ℃, ReCl 5molecular Adsorption is at carbon foam tube internal surface and decomposite rhenium atom, and rhenium atom is attached to carbon foam hole inwall equably, finally forms a kind of internal surface and be covered with the rhenium foam tube of rhenium metal layer.
4. preparation method according to claim 1, is characterized in that the concrete preparation process of described CVD iridium coating layer is: take praseodynium iridium as pioneer, at 180～250 ℃, make its volatilization, deposition occurs to decompose in the substrate that is heated to 500～600 ℃.
5. preparation method according to claim 1, is characterized in that the actual conditions of described electroformed nickel coating is: take nickelous sulfate as main salt, and 40～60 ℃ of temperature, direct current supply, current density is 1.0～3.0A/dm 2.
CN201310410630.1A 2013-09-11 2013-09-11 A kind of rhenium base refractory metal mixes the preparation method of pipe Active CN103727317B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
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
CN109550935A (en) * 2018-12-24 2019-04-02 中铼新材料有限公司 A kind of method of composite algorithm production 5N rhenium metal

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101787514A (en) * 2010-03-15 2010-07-28 南京航空航天大学 Platinum-group metal coating on surface of refractory metal and preparation method thereof
CN101899693A (en) * 2010-07-30 2010-12-01 安徽华东光电技术研究所 Method for locally plating rhenium on oxygen-free copper matrix
US20120156412A1 (en) * 2009-08-31 2012-06-21 Henkel Ag & Co. Kgaa Use of Low-Temperature Foamable Epoxide Resins in Hollow Chamber Structures
CN102548754A (en) * 2009-02-23 2012-07-04 金属泡沫技术有限公司 Metal tube with porous metal liner
CN102534290A (en) * 2012-03-06 2012-07-04 陈照峰 Platinum group metal alloy coating with controlled alloying elements and preparation method thereof
CN102847947A (en) * 2012-10-19 2013-01-02 广西梧州港德硬质合金制造有限公司 Sintering preparation method of hard alloy rings
CN103026419A (en) * 2010-06-16 2013-04-03 原子能与替代能源委员会 Solid interface joint with open porosity, for nuclear fuel rod
DE102011056418A1 (en) * 2011-12-14 2013-06-20 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Load-bearing reinforcement of internal pressure-loaded hollow bodies

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102548754A (en) * 2009-02-23 2012-07-04 金属泡沫技术有限公司 Metal tube with porous metal liner
US20120156412A1 (en) * 2009-08-31 2012-06-21 Henkel Ag & Co. Kgaa Use of Low-Temperature Foamable Epoxide Resins in Hollow Chamber Structures
CN101787514A (en) * 2010-03-15 2010-07-28 南京航空航天大学 Platinum-group metal coating on surface of refractory metal and preparation method thereof
CN103026419A (en) * 2010-06-16 2013-04-03 原子能与替代能源委员会 Solid interface joint with open porosity, for nuclear fuel rod
CN101899693A (en) * 2010-07-30 2010-12-01 安徽华东光电技术研究所 Method for locally plating rhenium on oxygen-free copper matrix
DE102011056418A1 (en) * 2011-12-14 2013-06-20 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Load-bearing reinforcement of internal pressure-loaded hollow bodies
CN102534290A (en) * 2012-03-06 2012-07-04 陈照峰 Platinum group metal alloy coating with controlled alloying elements and preparation method thereof
CN102847947A (en) * 2012-10-19 2013-01-02 广西梧州港德硬质合金制造有限公司 Sintering preparation method of hard alloy rings

Cited By (2)

* Cited by examiner, † Cited by third party
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
CN109550935A (en) * 2018-12-24 2019-04-02 中铼新材料有限公司 A kind of method of composite algorithm production 5N rhenium metal

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