CN101787514A - Platinum-group metal coating on surface of refractory metal and preparation method thereof - Google Patents
Platinum-group metal coating on surface of refractory metal and preparation method thereof Download PDFInfo
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- CN101787514A CN101787514A CN 201010123869 CN201010123869A CN101787514A CN 101787514 A CN101787514 A CN 101787514A CN 201010123869 CN201010123869 CN 201010123869 CN 201010123869 A CN201010123869 A CN 201010123869A CN 101787514 A CN101787514 A CN 101787514A
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Abstract
The invention provides a platinum-group metal coating 30 for refractory metal 10; a 0.2 to 2mu m transition layer 20 is arranged between the platinum-group metal coating 30 and the refractory metal base material 10; in the transition layer 20, from one side of the base material of the refractory metal 10 to one side of the platinum-group metal coating 30, the platinum-group metal elements are sequentially increased until the transition layer 20 ends, the content of the platinum-group metal elements reaches 100 percent, and the thickness of the platinum-group metal coating 30 is within 100mu m. The invention provides a method of preparing the platinum-group metal coating 30 on the surface of the refractory metal 10. The method is carried out in a vacuum furnace, uses platinum-group metal as a target, the target voltage is between 0 and -1200V, the refractory metal serves as the base material, and the voltage is between 0 and -900V. Argon serves as the working atmosphere, when the vacuum indoor pressure reaches 15 to 55Pa, a DC power supply is connected, and finally the platinum-group metal coating with preferred growth orientation is finally formed through continuous sputtering and anti-sputtering, absorption and desorption.
Description
Technical field
The present invention relates to a kind of platinum metals coating and preparation method thereof, especially relate to platinum metals coating of a kind of refractory metal surfaces and preparation method thereof.
Background technology
In various materials, refractory metal is the hyperthermal material of studying the earliest and being applied.What general Study and application were maximum mainly is refractory metals such as Nb, Mo, W, Re.Refractory metal has been widely used in aspects such as various spacecrafts and engine.Refractory metal has excellent hot strength, erosion resistance and performance such as high temperature resistant, but can make material failure because of oxidation in time more than 1000 ℃, has influenced the development of refractory metal material.Adopt platinum metals coating (iridium, platinum, ruthenium, rhodium, osmium, palladium) to improve the high-temperature oxidation resistance of refractory metal, become the candidate material that people pay close attention to as platinum, iridium.The platinum metals has high-melting-point, good chemical stability and good resistance of oxidation etc.Prepare the deficiency that the platinum metals coating then can remedy the refractory metal high-temperature oxidation resistance in refractory metal surfaces, the advantage of performance matrix itself and platinum metals coating.
The research to the platinum metals coating abroad starts to walk early, and wherein the research with the U.S., Russia, Japan is in world lead level.Research in China's platinum metals coating also is in the starting stage, and particularly aspect the preparation of coating, China has only a few research unit such as Kunming precious metal institute, Northwestern Polytechnical University etc. to carry out research work.Adopt different processing methodes to prepare the platinum metals coating in refractory metal surfaces, these methods mainly comprise electroplating deposition, chemical Vapor deposition process (CVD).The electroplating deposition method is a research coating method relatively early; use aluminum oxide or plumbago crucible as electrolyzer; electrolytic solution is the sodium cyanide of 70% under the molten state and 30% potassium cyanide; in argon shield atmosphere deposit, the electrochemical parameter in the deposition process is indeterminate to coating associativity and successional influence.This method advantage is can prepare the big area coating and at complex construction parts surface deposited coatings; Deficiency is that coating stress is big, relatively poor with combining of matrix, coating preparation cost height, and electrolytic solution has severe toxicity.The seventies in 20th century, US Naval Research Laboratory adopts the depositing operation and the mechanism of CVD method research platinum metals coating.This method is to utilize the deposition source of the halogenide making coatings of platinum metals, with Ar, H
2, CO or mixed gas be carrier gases.Halogenide is as precursor, and sedimentation rate is low, and the coating of preparation has vesicular structure, and coating and matrix bond are poor.In recent years, the research that MOCVD prepares the platinum metals film gets more and more, the researchist attempts adopting multiple different organometallics to carry out the CVD test of platinum metals, and the more satisfactory deposition source of deposition effect is a methyl ethyl diketone platinum metals organic coordination compound at present.People such as Japan Goto study as the application of electrode materials at the platinum metals film.With diacetyl acetone platinum, praseodynium iridium is raw material, adopts the hot wall type type of heating to prepare platinum, iridium film.American National aviation and space travel office (NASA) use the MOCVD method to prepare platinum metals iridium coating layer/compound jet pipe of rhenium base.This method is to utilize the thermolysis of methyl ethyl diketone iridium to prepare iridium coating layer.The successful key that chemical Vapor deposition process prepares iridium coating layer/rhenium based composites depends on the optimal deposition parameter.These parameters mainly comprise: be deposited the material gas compound, substrate temperature, gas concentration, flow velocity and pressure, the set size of reaction chamber and coat-thickness etc.People such as the Ultramet company of the U.S., Lewis research centre and Harding use mocvd method successfully to prepare the platinum metals iridium coating layer.Just the Re/Ir/C-C ultrahigh-temperature matrix material of low-thrust is used for the engine promotion room, makes the inwall of promotion room with iridium, and at high temperature oxidation-resistance is extremely strong to discover iridium coating layer, and this Ir/Re structure can prolong 10～20s down at 2200 ℃.This method advantage be can prepare successive, fine and close, in conjunction with coating preferably.This method shortcoming is that sedimentation rate is slow, cost height, other impurity such as the common carbon containing of coating of gained to the difficult control of processing parameter.
Description of drawings
Fig. 1 is the structural representation of coating.
Fig. 2 be refractory metal base material 10 down, platinum metals target 4 is at last synoptic diagram.
Fig. 3 be refractory metal base material 10 last, platinum metals target 40 under synoptic diagram.
Fig. 4 be refractory metal base material 10 in the platinum metals 40 lateral synoptic diagram.
Fig. 5 is that a refractory metal base material 10 is at two platinum metals, 40 intermediary synoptic diagram.
Fig. 6 is that a platinum metals target 40 is at two refractory metal base materials, 10 intermediary synoptic diagram.
Fig. 7 be taper refractory metal base material 10 ' taper platinum metals target sleeve 40 ' in synoptic diagram.
Fig. 8 is a cylindrical refractory metal base material 10 ' at cylindrical platinum metals target tube 40 ' outer synoptic diagram.
Fig. 9 is the platinum metals Ir coating of refractory metal Mo surface deposition.
10 is refractory metal base materials, the 20th shown in the figure, transition layer, the 30th, and the platinum metals coating, the 40th, the platinum metals target, 10 ' be revolution build refractory metal base material, 40 ' be revolution build platinum metals target.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of platinum metals coating 30 for infusibility metal base 10, the transition layer 20 that has one 0.2～2 micron thickness between this platinum metals coating 30 and the refractory metal base material 10, in the transition layer from refractory metal base material 10 1 sides to platinum metals coating 30 1 sides, platinum group increases progressively successively, finish until transition layer, platinum group content reaches 100%, and platinum metals coat-thickness 30 is in 100 microns.In the transition layer 20, but refractory metal element and platinum group Individual existence promptly exist with simple substance blended form, also combinable form exists and promptly forms compound, also can be the form existence of simple substance and compound.The platinum metals coating comprises iridium coating layer, platinum coating, ruthenium coating, rhodium coatings, osmium coating, palladium coating, and iridium rhodium alloy coating, platinum iridium alloy coating, ruthenium iridium alloy coating, other metal alloys of platinum family.
Another technical problem that the present invention will solve provides the preparation method of a kind of above-mentioned platinum metals coating 30.Aforesaid method carries out in vacuum chamber, uses platinum metals 40 as target, target band volts DS, voltage range 0～-1200V between; Refractory metal base material 10 also is with volts DS, voltage range 0～-900V between; Use argon gas as work atmosphere, when vacuum indoor pressure reaches 15～55Pa, connect direct supply, target 40 surfaces and base material 10 surfaces produce discharge respectively and form aura, and quilt aura parcel separately, when enough hour of target 40 and base material 10 distances, two kinds of aura overlap and form plasma body, by plasma sputtering bombardment target 40 elements, the platinum metals atom is sputtered, and flies to refractory metal base material 10 surfaces, and the platinum metals atom that is deposited on refractory metal base material 10 surfaces is sputtered once more, through successive sputter and reverse sputtering, absorption and desorption form transition layer 20 at last and have the platinum metals coating 30 that preferential growth is orientated.
Provided by the inventionly prepare the platinum metals coating process, comprise following processing steps in sequence in refractory metal surfaces:
(1) before the coating deposition, refractory metal base material 10 surfaces is handled, polished with abrasive paper for metallograph and respectively with acetone or alcohol ultrasonic cleaning, dry then;
(2) refractory metal base material 10 is put into vacuum chamber with platinum metals target 40, regulates its spacing;
(3) use mechanical pump that vacuum chamber pressure is evacuated to below the 5Pa, re-use molecular pump and be evacuated to highest attainable vacuum, open the recirculated cooling water of vacuum chamber then;
(4) charge into argon gas to vacuum chamber, making office work air pressure is 15～55Pa;
(5) after the stable gas pressure, power-on slowly increases refractory metal base material 10 voltages;
(6) rising platinum metals target 40 voltages and refractory metal base material 10 voltages cause the sputter of platinum metals target 40 elements, and produce stable plasma body;
(7) stable coatings preparation condition and time;
(8) slowly reduce voltage, powered-down, stop air feed, closure molecule pump, mechanical pump are cooled to room temperature, close water coolant, take out base material.
In above-mentioned coating production, it is characterized in that refractory metal base material 10 and platinum metals target 40 prepare transition layer 20 and platinum metals coating 30.
In above-mentioned coating production, it is characterized in that refractory metal base material 10 is under platinum metals target 40.
In above-mentioned coating production, it is characterized in that refractory metal base material 10 is on platinum metals target 40.
In above-mentioned coating production, it is characterized in that refractory metal base material 10 is between two platinum metals targets 40.
In above-mentioned coating production, it is characterized in that a platinum metals target 40 is between two refractory metal base materials 10.
In above-mentioned coating production, it is characterized in that in refractory metal base material solid of revolution 10 ' surfaces externally and internally and platinum metals solid of revolution target 40 ' prepare transition layer 20 and platinum metals coating 30.
In above-mentioned coating production, it is characterized in that platinum metals target solid of revolution 40 ' refractory metal base material solid of revolution 10 ' outside.
In above-mentioned coating production, it is characterized in that platinum metals target solid of revolution 40 ' refractory metal base material solid of revolution 10 ' within.
In above-mentioned coating production, it is characterized in that preparing in the coating procedure, distance is between 5～30mm between platinum metals target 40 and the refractory metal base material 10.
In above-mentioned coating production, it is characterized in that the thickness of the thickness of transition layer 20 and platinum metals coating 30 and crystal preferred orientation can be by adjusting processing parameters controls such as refractory metal base material voltage, platinum metals target voltage, soaking time.
In above-mentioned coating production, it is characterized in that refractory metal base material 10 absolute value of voltage are lower than platinum metals target 40 absolute value of voltage.
In above-mentioned coating production, it is characterized in that refractory metal base material solid of revolution 10 ' absolute value of voltage is lower than platinum metals target solid of revolution 40 ' absolute value of voltage.
According to above-mentioned technological process, it is characterized in that giving earlier the refractory metal base material 10 energisings, give the platinum metals target 40 energisings then.
According to above-mentioned technological process, it is characterized in that giving earlier refractory metal base material solid of revolution 10 ' energising, give platinum metals target solid of revolution 40 ' energising then.
According to above-mentioned technological process, it is characterized in that 10 energisings of refractory metal base material and the timed interval of platinum metals target 40 energisings are 0～30 minute.
According to above-mentioned technological process, it is characterized in that the refractory metal base material solid of revolution 10 ' energising and the timed interval of platinum metals target solid of revolution 40 ' energising are 0～30 minute.
The invention has the advantages that: (1) sedimentation velocity is fast, and thickness is controlled easily, has improved the efficient of platinum metals coating preparation; (2) refractory metal basal body to curve form also can prepare the platinum metals coating; (3) can obtain smooth, bright and clean, fine and close successive platinum metals coating; (4) the platinum metals coating is divided into transition layer and settled layer two portions, and transition layer is positioned at the refractory metal specimen surface, combines good between noble coatings and the refractory metal.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
The refractory metal molybdenum plate is of a size of 15mm * 15mm * 2mm as base material; Platinum metals iridium plate is of a size of as target
The refractory metal specimen surface is handled, polished with abrasive paper for metallograph and respectively with acetone or alcohol ultrasonic cleaning, dries afterwards.Good at the vacuum indoor set, regulate interpole gap, feed argon gas after being evacuated to highest attainable vacuum.Setting the processing parameter that adopts present technique to prepare the platinum metals iridium coating layer on the refractory metal molybdenum base material is: target voltage is-850V; Base material voltage is-300～-350V, operating air pressure 35Pa, iridium target and molybdenum base material spacing 15mm, depositing time 2h.Molybdenum base material voltage is adjusted to earlier-450V, opens the target power supply after 15 minutes again, carry out the deposition of coating according to the above-mentioned processing parameter that configures, temperature can reach 900-1000 ℃ in the deposition process.Higher temperature helps iridium coating layer and combines with the base material elemental diffusion, forms in conjunction with good iridium coating layer.Fig. 9 is the cross section microstructure photograph of deposition iridium coating layer on the molybdenum base material.Sedimentary iridium coating layer thickness is 7 μ m on the molybdenum, and the coating average sedimentation rate reaches 3.5 μ m/h.Sample and matrix the thick transition layer of about 0.7 μ m appears at the interface, transition layer can strengthen combining between coating and the matrix.Coating is the most surperficial to confirm that by electronic spectrum platinum metals iridium content reaches 100%.
Embodiment 2
Using the refractory metals tungsten sample as base material, is target with 70% iridium+30% platinum alloy powder metallurgy dish.The refractory metals tungsten substrate surface is handled, polished with abrasive paper for metallograph and respectively with acetone or alcohol ultrasonic cleaning, dries afterwards.Good at the vacuum indoor set, regulate interpole gap, feed argon gas after being evacuated to highest attainable vacuum.The deposition process parameters of base material: operating air pressure 45Pa, target current potential are-900V that the base material current potential is-450V that interpole gap is 13mm.Earlier base material voltage is adjusted to-550V, regulate base material behind the 20min and target voltage be respectively-450V ,-900V.Through the 2h deposition, can obtain the thick fine and close platinum iridium alloy coating of 15 μ m, transition region thickness is about 0.9 μ m.The layering peeling phenomenon does not appear in the platinoiridita coating of preparation, combines better with refractory metals tungsten.
Claims (10)
1. the present invention provides a kind of platinum metals coating for refractory metal, has a transition layer between this platinum metals coating and the refractory metal base material, in the transition layer from refractory metal base material one side to platinum metals coating one side, platinum group increases progressively successively, finish until transition layer, platinum group content reaches 100%.
2. described according to claim 1, it is characterized in that transition region thickness is 0.2～2 micron, the platinum metals coat-thickness is in 100 microns.
3. described according to claim 1, it is characterized in that in the transition layer that refractory metal element and platinum group exist with simple substance blended form, exist with the bonded form, the form of all right simple substance and compound exists.
4. described according to claim 1, it is characterized in that the platinum metals coating comprises iridium coating layer, platinum coating, ruthenium coating, rhodium coatings, osmium coating, palladium coating, iridium rhodium coatings, platinoiridita coating, ruthenium iridium coating layer, other metal alloy coatings of platinum family.
5. be used to prepare the method for the described coating of claim 1, it is characterized in that carrying out in vacuum oven, all logical direct current of target and base material comprises following processing steps in sequence:
(1) before the coating deposition, the refractory metal substrate surface is handled, polished with abrasive paper for metallograph and respectively with acetone or alcohol ultrasonic cleaning, dries then;
(2) refractory metal base material and platinum metals target are put into vacuum chamber, regulate its spacing;
(3) use mechanical pump that vacuum chamber pressure is evacuated to below the 5Pa, re-use molecular pump and be evacuated to highest attainable vacuum, open the recirculated cooling water of vacuum chamber then;
(4) charge into argon gas to vacuum chamber, making office work air pressure is 15～55Pa;
(5) after the stable gas pressure, power-on slowly increases refractory metal base material voltage;
(6) rising platinum metals target voltage and refractory metal base material voltage cause the sputter of platinum metals target elements, and produce stable plasma body;
(7) stable coatings preparation condition and time;
(8) slowly reduce voltage, powered-down, stop air feed, closure molecule pump, mechanical pump are cooled to room temperature, close water coolant, take out base material.
6. described according to claim 5, it is characterized in that refractory metal base material and platinum metals target can be tabulars, also can be solid of revolution.
7. described according to claim 5, it is characterized in that the refractory metal base material is under the target of platinum metals, also but the refractory metal base material is on the target of platinum metals, also can a refractory metal base material between two platinum metals targets, also can a platinum metals target between two refractory metal base materials.
8. described according to claim 5, it is characterized in that refractory metal base material voltage 0～-900V between, platinum metals target voltage 0～-1200V between, refractory metal base material absolute value of voltage is lower than platinum metals target absolute value of voltage in the coating preparation process, give the energising of refractory metal base material earlier, give platinum metals target energising then, the timed interval is 0～30 minute.
9. described according to claim 5, it is characterized in that in the coating preparation process that distance is between 5～30mm between platinum metals target and the refractory metal base material.
10. described according to claim 5, the thickness that it is characterized in that transition layer is by adjusting refractory metal base material voltage and platinum metals target voltage control.
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| CN102534290A (en) * | 2012-03-06 | 2012-07-04 | 陈照峰 | Platinum group metal alloy coating with controlled alloying elements and preparation method thereof |
| CN102899614A (en) * | 2012-07-16 | 2013-01-30 | 南京航空航天大学 | High temperature stable spark plug electrode coating and preparation method |
| CN102991021A (en) * | 2012-12-14 | 2013-03-27 | 南京航空航天大学 | Ultrahigh-temperature anti-oxidation composite coating and preparation method thereof |
| CN103524033A (en) * | 2012-07-06 | 2014-01-22 | 苏州宏久航空防热材料科技有限公司 | High-temperature alloy bushing plate plated by platinum and alloy thereof, and preparation method of high-temperature alloy bushing plate |
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| CN102899614A (en) * | 2012-07-16 | 2013-01-30 | 南京航空航天大学 | High temperature stable spark plug electrode coating and preparation method |
| CN102991021A (en) * | 2012-12-14 | 2013-03-27 | 南京航空航天大学 | Ultrahigh-temperature anti-oxidation composite coating and preparation method thereof |
| CN104376952A (en) * | 2013-08-12 | 2015-02-25 | 苏州宏久航空防热材料科技有限公司 | Platinum-alloy-plated high-temperature alloy iron core |
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| CN103738001B (en) * | 2013-09-11 | 2016-01-13 | 太仓派欧技术咨询服务有限公司 | A kind of rhenium base refractory metal hybrid materials and structure thereof |
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| CN106013593A (en) * | 2016-06-08 | 2016-10-12 | 安徽汇力建筑工程有限公司 | High-density fiberboard and oriented strand board composite structure wallboard |
| CN106013590A (en) * | 2016-06-08 | 2016-10-12 | 安徽汇力建筑工程有限公司 | Light thermal insulation curtain wall material |
| CN106013593B (en) * | 2016-06-08 | 2018-05-01 | 安徽汇力建筑工程有限公司 | A kind of high density fiberboard and oriented wood chipboard composite construction wallboard |
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| CN106013590B (en) * | 2016-06-08 | 2018-05-04 | 安徽汇力建筑工程有限公司 | A kind of light thermal-insulation curtain wall material |
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| CN111441024A (en) * | 2020-04-29 | 2020-07-24 | 金堆城钼业股份有限公司 | Tungsten surface oxygen-blocking film and preparation method thereof |
| CN112030231A (en) * | 2020-08-28 | 2020-12-04 | 北京中材人工晶体研究院有限公司 | Composite material and preparation method and application thereof |
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