CN102534617B - Method for preventing molybdenum and molybdenum alloys from being oxidized - Google Patents
Method for preventing molybdenum and molybdenum alloys from being oxidized Download PDFInfo
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- CN102534617B CN102534617B CN2012100394767A CN201210039476A CN102534617B CN 102534617 B CN102534617 B CN 102534617B CN 2012100394767 A CN2012100394767 A CN 2012100394767A CN 201210039476 A CN201210039476 A CN 201210039476A CN 102534617 B CN102534617 B CN 102534617B
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000011733 molybdenum Substances 0.000 title claims abstract description 66
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 65
- 229910001182 Mo alloy Inorganic materials 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000010936 titanium Substances 0.000 claims abstract description 59
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 43
- 239000000956 alloy Substances 0.000 claims abstract description 16
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 13
- 230000003064 anti-oxidating effect Effects 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 239000011159 matrix material Substances 0.000 claims description 33
- 239000000843 powder Substances 0.000 claims description 32
- 238000000576 coating method Methods 0.000 claims description 27
- 239000011248 coating agent Substances 0.000 claims description 25
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 19
- 230000003647 oxidation Effects 0.000 claims description 19
- 238000007254 oxidation reaction Methods 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 13
- 238000012545 processing Methods 0.000 claims description 12
- 239000007921 spray Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 10
- 239000010931 gold Substances 0.000 claims description 10
- 229910052737 gold Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910000858 La alloy Inorganic materials 0.000 claims description 9
- CBPOHXPWQZEPHI-UHFFFAOYSA-N [Mo].[La] Chemical compound [Mo].[La] CBPOHXPWQZEPHI-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- 229910000691 Re alloy Inorganic materials 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 4
- 238000010410 dusting Methods 0.000 claims description 4
- 229960004756 ethanol Drugs 0.000 claims description 4
- 230000004927 fusion Effects 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- YUSUJSHEOICGOO-UHFFFAOYSA-N molybdenum rhenium Chemical compound [Mo].[Mo].[Re].[Re].[Re] YUSUJSHEOICGOO-UHFFFAOYSA-N 0.000 claims description 4
- 238000007747 plating Methods 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000000280 densification Methods 0.000 claims description 3
- 238000002161 passivation Methods 0.000 claims description 3
- 229910017315 Mo—Cu Inorganic materials 0.000 claims description 2
- 244000137852 Petrea volubilis Species 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 238000005137 deposition process Methods 0.000 claims description 2
- 238000007772 electroless plating Methods 0.000 claims description 2
- 239000008151 electrolyte solution Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 238000004381 surface treatment Methods 0.000 claims description 2
- 238000007738 vacuum evaporation Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 238000007780 powder milling Methods 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 3
- 238000005275 alloying Methods 0.000 description 2
- 230000006399 behavior Effects 0.000 description 2
- 229910000951 Aluminide Inorganic materials 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910000753 refractory alloy Inorganic materials 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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Abstract
The invention provides a method for preventing molybdenum and molybdenum alloys from being oxidized and belongs to a method for antioxidation treatment on surface of the alloys. According to the method, the surfaces of molybdenum and molybdenum alloys are treated by titanium, the titanium contacts oxygen to form a layer of dense titanium oxide film to passivate the surface of molybdenum and molybdenum alloys, and thus, the molybdenum and molybdenum alloys are prevented from being oxidized. According to the method, through the surface titanium treatment, the molybdenum and molybdenum alloys can be prevented from being oxidized; and the film has high compatibility with molybdenum and molybdenum alloy substrates, high heat resistance and other advantages, and expands the application range of molybdenum and molybdenum alloys.
Description
Technical field
The present invention relates to a kind of method that alloy surface is processed, particularly a kind of method that prevents molybdenum and molybdenum alloy oxidation of processing by surperficial titanium.
Background technology
Molybdenum and molybdenum alloy are a kind of important superalloys, because it has the advantages such as high-melting-point, anticorrosive, mechanical property is excellent, thereby in fields such as thermal structure part, aerospace industry, nuclear power industry, electronic industry and glass works, purposes are widely arranged.But, due to molybdenum and molybdenum alloy, form MoO approximately oxidation can occurring 300 ℃ the time
2, secondary oxidation can occur during ℃ left and right in temperature rise to 600, generates MoO
3, when temperature rises to 750 ℃ and when above, MoO
3serious volatilization is yellow smog.So the oxidation of molybdenum and volatilization phenomenon have affected its mechanical behavior under high temperature, have limited the range of application of molybdenum and molybdenum alloy.
The approach that solves at present molybdenum and molybdenum alloy oxidisability has two, and the one, the molybdenum alloy of development high-temperature oxidation resistant, the 2nd, additional oxidation resistant coating.But but the alloying level of molybdenum is very little, when the alloy adding that improves antioxidant property is slightly many, the poor processability of alloy, very the person does not have temperature-room type plasticity, so can't fundamentally change the resistance of oxidation of molybdenum and molybdenum alloy by the method for alloying, but also can have influence on its many high-temperature behaviors, as hot strength, shock-resistance, resistance to heat shocks and creep resistance etc.So, prepare coating on the surface of molybdenum and molybdenum alloy and prevent that oxidation just seems very necessary.Common high-temperature oxidation resistant coating has aluminide coating, silicide coating, refractory alloy coating, noble coatings etc., but mostly has the shortcomings such as coating and substrate combinating strength are not high, consistency is poor, high cost (noble coatings).
Summary of the invention
Defect or deficiency for existing anti-oxidation technology, the object of the invention is to, and proposes a kind of method that prevents molybdenum and molybdenum alloy oxidation of processing by surperficial titanium.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of method that prevents molybdenum and molybdenum alloy oxidation, it is characterized in that, at first the method carries out surface treatment to molybdenum and molybdenum alloy matrix, then carry out the titanium processing at surface treated molybdenum and molybdenum alloy matrix surface, titanium with after oxygen contacts on the molybdenum alloy matrix chemical combination generate the oxidation titanium film of one deck densification, make molybdenum and molybdenum alloy surface passivation, with this, prevent the oxidation of molybdenum and molybdenum alloy.
The above-mentioned body material for anti-oxidation can be that pure molybdenum, Mo-Ti are associated gold, Mo-W and are associated gold, Mo-Cu and are associated that gold, Mo-Re are associated gold, Mo-Hf-C is associated gold, TZC alloy, TZM alloy etc.
The method that above-mentioned surperficial titanium is processed adopts thermospray, electroless plating, physical vacuum vapour deposition plating, chemical gas phase plating or vacuum evaporation coating etc.
The use temperature of above-mentioned molybdenum after surperficial titanium is processed and molybdenum alloy≤1200 ℃.
The present invention processes and prevents molybdenum and molybdenum alloy oxidation by surperficial titanium, compared with prior art has the following advantages:
1. can realize by number of ways the titanium processing of molybdenum and molybdenum alloy surface;
2. molybdenum and the molybdenum alloy thermotolerance after surperficial titanium processing is high;
3. to carry out the consistency of titanium processing and molybdenum and molybdenum alloy matrix good on surface.
The accompanying drawing explanation
Energy spectrogram and the elemental composition table of the sealer of pure molybdenum after surperficial titanium is processed in Fig. 1: embodiment 1;
Can spectrogram and elemental composition table after the surface protection layer segment polishing of pure molybdenum after surperficial titanium is processed in Fig. 2: embodiment 1;
In Fig. 3: embodiment 1 sealer of pure molybdenum after surperficial titanium is processed polish fully after material internal energy spectrogram and elemental composition table;
Metallographic structure in Fig. 4: embodiment 1 after surperficial titanium is processed.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment
The mechanism that the present invention adopts is, titanium and molybdenum belong to rare refractory metal together, fusing point is high, titanium and titanium oxide all have good thermotolerance, good with molybdenum and molybdenum alloy matrix phase capacitive, carry out the titanium processing at molybdenum and molybdenum alloy surface, after titanium contacts with oxygen, chemical combination generates the oxidation titanium film of one deck densification, in the time of can eliminating high temperature, oxygen and molybdenum and molybdenum alloy matrix contacts, thereby reduced the diffusion of oxygen to the molybdenum matrix, it has arrived the effect of surface passivation, reached the purpose that prevents molybdenum and the oxidation of molybdenum alloy matrix, improved the work-ing life of molybdenum and molybdenum alloy material, enlarged the use range of molybdenum and molybdenum alloy.
Below the embodiment that the contriver provides:
Embodiment 1:
The energy spectrogram of the sealer after surperficial titanium is processed and elemental composition table are as shown in Figure 1; after surface protection layer segment polishing after surperficial titanium is processed, energy spectrogram and elemental composition table are as shown in Figure 2; sealer after surperficial titanium is processed polish fully after material internal can spectrogram and the elemental composition table as shown in Figure 3, the metallographic structure after surperficial titanium is processed is as shown in Figure 4.
Embodiment 2:
Embodiment 3:
Embodiment 4:
Embodiment 5:
Embodiment 6:
Embodiment 7:
Through applicant's detection, the use temperature of above molybdenum after surperficial titanium is processed and molybdenum alloy≤1200 ℃.
Above-described embodiment is preferably example of the present invention; only for the present invention is described; the invention is not restricted to above-described embodiment, the interpolation of every technical characterictic of doing according to the technical scheme of the technology of the present invention, equivalent transformation, all belong to the protection domain of technical solution of the present invention.
Claims (1)
1. a method that prevents molybdenum and molybdenum alloy oxidation, it is characterized in that, at first the method carries out surface treatment to molybdenum and molybdenum alloy matrix, then carry out the titanium processing at surface treated molybdenum and molybdenum alloy matrix surface, titanium with after oxygen contacts on the molybdenum alloy matrix chemical combination generate the oxidation titanium film of one deck densification, make molybdenum and molybdenum alloy surface passivation;
Described molybdenum and molybdenum alloy body material are that pure molybdenum, Mo-Ti are associated gold, Mo-W and are associated gold, Mo-Cu and are associated that gold, Mo-Re are associated gold, Mo-Hf-C is associated gold, TZC alloy or TZM alloy;
The method that described surperficial titanium is processed is thermospray, electroless plating, physical vacuum vapour deposition plating, chemical gas phase plating or vacuum evaporation coating;
Molybdenum after surperficial titanium is processed and the use temperature of molybdenum alloy≤1200 ℃;
Specifically follow these steps to carry out:
Step 1, choosing purity is the pure molybdenum more than 99.95%, with dipping in the alkalis of 25g/L 30 minutes, with 90 ℃ of distilled water cleanings 40 minutes, then uses 40 ℃ of clear water spray washings drying for standby after a hour;
Step 2, prepare coated powder, and the mesh screen that is 50 μ m with sieve aperture sieves out TiO
2powder, drying for standby;
Step 3, adopt electrostatic powder spraying to carry out surperficial titanium processing, and the amount of dusting is that 50g/ divides, spray time is 10s, repeats to spray 6 times, and the voltage that dusts is 60V, fusion bonded temperature is 538 ℃, and the clinkering time is 12 minutes, after furnace cooling, on pure molybdenum surface, forms fine and close TiO
2film;
Perhaps:
Step 1, choose the molybdenum-lanthanum alloy matrix, through sanding and polishing, to minute surface, through ultrasonic cleaning, is put in dehydrated alcohol standby;
Step 2, prepare coated powder, and purity is 99.9%, 200 purpose TiO
2with pure Ti powder, both mass ratioes are 0.45; Ball milling 60 minutes, dry for standby;
Step 3, the preparation coating, adopt vapour deposition method to carry out surperficial titanium processing, and evaporate process is carried out in SL63-7B type vacuum resistance furnace, and vacuum tightness is 0.9 * 10
-2pa; Molybdenum-lanthanum alloy is imbedded to TiO
2in the mixture of powder and pure Ti powder, be heated to 650 ℃, be incubated 2 hours, after furnace cooling, on the molybdenum-lanthanum alloy surface, form fine and close anti-oxidation TiO
2film;
Perhaps:
Step 1, choose the TZM alloy substrate, and surface is put in dehydrated alcohol standby after cleaning with ethanol;
Step 2, configuration fused salt, MgCl
2, NaCl, BaCl
2ratio in 1.1:1:2 is mixed, and then sneaks into 200 order Ti powder, and ball milling, after 2 hours, is put into crucible standby;
Step 3, imbed the molybdenum alloy matrix in crucible, with salt and Ti powder mixture, covers and compacting, be heated to 750 ℃, sintering, after 20 minutes, is put into 100 ℃ of environment dry 2 hours, cooling screening, obtain titanium and process the TZM alloy material that there is fine and close anti-oxidation Ti layer rear surface;
Perhaps:
Step 1, choose molybdenum rhenium alloys matrix, first by 260#SiO
2, 1000#SiC, 1500#SiC sand paper be polished to minute surface, puts into distilled water and carry out ultrasonic cleaning, after taking-up, is kept in dehydrated alcohol standby;
Step 2, metallic titanium powder 300 order purity are 99.9%, TiO
2powder is analytical pure, and both press the 1:1 mixing, and ball milling is standby after 2 hours;
Step 3, the preparation coating, evaporate process is carried out in SL63-7B type vacuum resistance furnace, and vacuum tightness is 1.2 * 10
-2pa; Molybdenum rhenium alloys matrix is imbedded to TiO
2in powder and pure Ti powder mixture, be heated to 950 ℃, be incubated 2 hours, after furnace cooling, at molybdenum rhenium alloys matrix surface, form fine and close TiO
2film;
Perhaps:
Step 1, choosing purity is the pure molybdenum more than 99.95%, through sanding and polishing, to minute surface, through ultrasonic cleaning, is put in dehydrated alcohol standby;
Step 2, prepare coated powder, and the mesh screen that is 50 μ m with sieve aperture sieves out TiO
2powder, drying for standby;
Step 3, adopt electrostatic powder spraying to prepare coating, and the amount of dusting is that 35g/ divides, and spray time is 7s, repeats to spray 6 times, and the voltage that dusts is-45V, and fusion bonded temperature is 538 ℃, and the clinkering time is 12 minutes, after furnace cooling, at the molybdenum matrix surface, forms fine and close TiO
2film;
Perhaps:
Step 1, choose the TZM alloy substrate, and surface is put in dehydrated alcohol standby after cleaning with ethanol;
Step 2, prepare the coating titanium, selects 99.99% Ti powder, and the Ti Powder Particle Size is 6 μ m;
Step 3, prepare coating, adopts vapour deposition process, utilizes the EWC060 device, and coiling chamber vacuum tightness is 10
-4holder, deposited chamber is 2 * 10
-4holder; Power ratio control, at 100KVA, continues 16 minutes, forms the coating of 4-12 μ m thickness at the TZM alloy surface;
Perhaps:
Step 1, choose the molybdenum-lanthanum alloy matrix, with dipping in the alkalis of 25g/L 30 minutes, with 90 ℃ of distilled water cleanings 40 minutes, then uses 40 ℃ of clear water spray washings drying for standby after a hour;
Step 2, configure electrolytic solution, selects the Ti(OH of 100g/L)
4the aqueous solution, be mixed with HF content 250g/L, NH
4f content 50g/L, the solution of carpenter's glue content 2g/L, constant temperature is at 45 ℃;
Step 3, prepare galvanization coating, adopts the insoluble platinum anode, and voltage is 30V, electroplates after 30 minutes and form at the molybdenum-lanthanum alloy matrix surface coating that thickness is 1.0-5.6 μ m thickness.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100394767A CN102534617B (en) | 2012-02-21 | 2012-02-21 | Method for preventing molybdenum and molybdenum alloys from being oxidized |
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|---|---|---|---|
| CN2012100394767A CN102534617B (en) | 2012-02-21 | 2012-02-21 | Method for preventing molybdenum and molybdenum alloys from being oxidized |
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| CN103938190B (en) * | 2014-05-16 | 2016-04-06 | 西安建筑科技大学 | The preparation method of a kind of molybdenum and molybdenum alloy surface oxidation resistant coating |
| CN105385987B (en) * | 2015-10-15 | 2018-11-13 | 厦门理工学院 | Tungsten surface high-temp anti oxidation layer and preparation method thereof |
| CN105386013B (en) * | 2015-11-16 | 2017-11-10 | 西安建筑科技大学 | A kind of molybdenum or molybdenum alloy surface Pd CeO2The preparation method of Co nano coatings |
| CN107199342A (en) * | 2017-05-09 | 2017-09-26 | 中国科学院兰州化学物理研究所 | A kind of preparation method of Mo Re alloy powders |
| CN115710690A (en) * | 2022-11-30 | 2023-02-24 | 江苏伊斯达尔精密科技有限公司 | Oxidation-resistant cermet material and preparation method thereof |
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Effective date of registration: 20231113 Address after: Units 208-210 and 209-211, Zone E, Science and Technology Innovation Base, No. 80 Ranyue Road, Science City, Huangpu District, Guangzhou City, Guangdong Province, 510700 (office only) Patentee after: GUANGZHOU QIDA MATERIAL & TECHNOLOGY Co.,Ltd. Patentee after: GUANGDONG QIDA TECHNOLOGY Co.,Ltd. Address before: 710055 No. 13, Yanta Road, Shaanxi, Xi'an Patentee before: XIAN University OF ARCHITECTURE AND TECHNOLOG |
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