CN107858636A - The standby Al of powder heap control oxygen compacting2O3And Cr2O3The method of film - Google Patents
The standby Al of powder heap control oxygen compacting2O3And Cr2O3The method of film Download PDFInfo
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- CN107858636A CN107858636A CN201711002485.8A CN201711002485A CN107858636A CN 107858636 A CN107858636 A CN 107858636A CN 201711002485 A CN201711002485 A CN 201711002485A CN 107858636 A CN107858636 A CN 107858636A
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- film
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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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/60—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes
- C23C8/62—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes only one element being applied
-
- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
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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)
- Powder Metallurgy (AREA)
Abstract
The invention belongs to face coat paint-on technique, refers in particular to the standby Al of powder heap control oxygen compacting2O3And Cr2O3The method of film.Present invention utilizes a kind of new powder heap Fe FeO to control oxygen pressure, and Al is prepared with seldom addition element under low oxygen pressure2O3And Cr2O3Film, regulation oxygen pressure can obtain pure Al2O3Or Cr2O3Or both mixing, far less than preparing Al in an atmosphere2O3And Cr2O3Al, Cr content of addition needed for film.Oxygen pressure, safer saving are controlled compared to gas is passed through.This powder heap composition will not also evaporate, and be vaporized on alloy surface and undergone phase transition with matrix.
Description
Technical field
Patent of the present invention belongs to face coat paint-on technique, and in particular to Al, Cr alloy containing active element are in low oxygen pressure
Under the conditions of selective oxidation occurs there is the preparation method of high temperature oxidation resistance film in Surface Creation.
Background technology
Metal is wide variety of material, is usually added into a large amount of alloying elements (Cr, Al, Si, Mn, Re) to improve high temperature
Anti-oxidant and normal temperature corrosion resistance.Selective oxidation will be occurred by being heated at high temperature these elements in an atmosphere, be formed on surface
Fine and close oxide-film and be protected material surface, this is also the oxidation resistant essence of high temperature alloy.But caused to be formed
Close selective oxidation film, it is necessary to add enough alloying elements, other performance can be caused to deteriorate, also make material cost increase.
Under the conditions of low oxygen pressure, alloying element is to surface enrichment, and a small amount of alloying element can forms fine and close selective oxidation in material
Film, this tunic can effectively prevent further being corroded for alloy, and the requirement of alloying element addition is declined to a great extent, makes material
Design has more flexibility.Such as Fe-Al alloys, to form pellumina, A1 contents must high temperature：＞ 12%；Room temperature:＞
6%.And under 77K dew points, Fe -5Al can form pellumina at high temperature.For Fe-Cr-Al base electrothermal alloys, to protect
Card alloy has preferable mechanical property, and w (Al) should be controlled within 16%, and this requires that Fe-Cr-Al alloys must contain foot
Enough chromium w (Cr) (18%~27%), it just can guarantee that to form the Al of densification2O3Film and be protected alloy.And in 0.1Mpa
Under, Fe-5Cr-5Al can also form one layer of alumina layer.
The pre-oxidation film formed using selective oxidation principle is also improved corrosion resistance and suppression in follow-up work environment
The ability of catalytic coking, and selective oxide film is combined with matrix better than the oxide-film formed in atmosphere, it is more smooth, airtight
Property is more preferable.Artificial manufacture low oxygen pressure generally has 2 kinds of methods, passes through powder heap (metal and its oxide powder) in vacuum tank
Or gas is passed through into vacuum tank, such as H2、H2O、O2、N2、CO2、 CO.Selective oxidation is divided into internal oxidition and external oxidation again, when
When oxygen forces down, the diffusion velocity of element is faster than the diffusion velocity of oxygen, and the alloying element and oxygen for first diffusing to surface occur instead
Should, in Surface Creation oxide；When oxygen pressure is high, oxygen first reaches sub-surface layer, occurs with the reactive alloys element in steel anti-
Should, generate oxide in sub-surface.
The content of the invention
It is an object of the invention to provide one kind to prepare pure Al2O3, pure Cr2O3With the new method of both mixed oxidization films.
Compact and complete protective oxide film is formed on surface with less addition element, economized on resources, makes design of material more flexible.
A kind of described standby Al of powder heap control oxygen compacting2O3And Cr2O3The method and step of film is as follows：
(1) after vacuum arc melting alloy in vacuum atmosphere homogenizing annealing 1 week.
(2) the sample section after annealing, is polished after grinding off surface scale, and surface is removed through alcohol and acetone cleaning
Impurity and greasy dirt.
(3) Fe-FeO powder heaps are put into quartz ampoule, depression will be burnt by then vacuumizing in the middle part of quartz ampoule, in the middle part of quartz ampoule not
Closure, atmosphere circulates while the alloy is separated with powder heap, as shown in Figure 1.Overall was hollow circuit cylinder originally, and centre is burnt
Fall in, alloy is contacted with powder heap, powder will not be sprinkled upon on alloy, but can not be closed completely, after quartz ampoule cooling
It is put into and places into alloy and vacuumize sealing.
(4) heating-up temperature of Fe-FeO powder heaps is set in the range of 800~900 DEG C, Po2=10-17~10-20Atm, electricity
The heating temperature range of arc molten alloy is 900~1000 DEG C, and insulation 1h can be obtained by complete pure Al2O3, pure Cr2O3Or
Both mixed layers.
Fe and FeO mass ratio is 1 in the Fe-FeO powder heaps:1.
The alloy is ferrous alloy, and Al, Cr are contained in ferrous alloy vivaciously and fine and close protective can be formed on surface
Oxide-film；Al content 3wt.%, Cr content 4-6wt.%.
The technical characteristic that the present invention is different from prior art is to make use of a kind of new powder heap Fe-FeO to control oxygen pressure,
Al is prepared with seldom addition element under low oxygen pressure2O3And Cr2O3Film, regulation oxygen pressure can obtain pure Al2O3Or Cr2O3Or two
The mixing of person, far less than preparing Al in an atmosphere2O3And Cr2O3Al, Cr content of addition needed for film.Compared to being passed through gas
Body controls oxygen pressure, safer saving.This powder heap composition will not also evaporate, and be vaporized on alloy surface and undergone phase transition with matrix.
Brief description of the drawings
Fig. 1 is the quartz ampoule schematic diagram after vacuum sealing.
Fig. 2 is 800 DEG C of (Po of powder heap2=10-19Atm), (a) surface after 950 DEG C of heating 1h of Fe-3Al-4Cr alloys；
(b) section.
Fig. 3 is 800 DEG C of (Po of powder heap2=10-19Atm), (a) surface after 950 DEG C of heating 1h of Fe-3Al-6Cr alloys；
(b) section.
Fig. 4 is 860 DEG C of (Po of powder heap2=10-17Atm), the surface after 1000 DEG C of heating 1h of Fe-3Al-6Cr alloys.
Fig. 5 is (a) surface after 1h of the sample after 800 DEG C of oxidation 50h；(b) section.
Embodiment
Embodiment 1：
(1) electric arc melting Fe-3Al-4Cr alloys, homogenizing annealing 1 week in vacuum atmosphere；
(2) sample after annealing is cut into the thin slice after 1mm, is polished after grinding off surface scale, is cleaned through alcohol and acetone
Remove the impurity and greasy dirt on surface.
(3) by Fe-FeO powder heaps (mass ratio 1:1) quartz ampoule is put into, depression will be burnt by then vacuumizing in the middle part of quartz ampoule
(not closing in the middle part of quartz ampoule, atmosphere circulates while the alloy is separated with powder heap), is put into after quartz ampoule cooling and places into
Alloy vacuumizes sealing；
(4) quartz ampoule is put into dual temperature tube furnace, the heating-up temperature of powder heap is 800 DEG C (10-19Atm), alloy plus
Hot temperature is 950 DEG C, heats 1h jointly, you can pure Cr is formed on surface2O3Film, as shown in Figure 2.
Embodiment 2：
(1) electric arc melting Fe-3Al-6Cr alloys, homogenizing annealing 1 week in vacuum atmosphere；
(2) sample after annealing is cut into the thin slice after 1mm, is polished after grinding off surface scale, is cleaned through alcohol and acetone
Remove the impurity and greasy dirt on surface；
(3) by alloy and Fe-FeO powder heaps (mass ratio 1:1) it is sequentially placed into quartz ampoule and is pumped into container with vavuum pump
Sealed after high vacuum；
(4) quartz ampoule is put into dual temperature tube furnace, the heating-up temperature of powder heap is 800 DEG C (10-19Atm), alloy plus
Hot temperature is 950 DEG C, heats 1h jointly, you can forms Al on surface2O3、Cr2O3Hybrid films, as shown in Figure 3.
Embodiment 3：
(1) electric arc melting Fe-3Al-6Cr alloys, homogenizing annealing 1 week in vacuum atmosphere；
(2) sample after annealing is cut into the thin slice after 1mm, is polished after grinding off surface scale, is cleaned through alcohol and acetone
Remove the impurity and greasy dirt on surface；
(3) by Fe-FeO powder heaps (mass ratio 1:1) quartz ampoule is put into, depression will be burnt by then vacuumizing in the middle part of quartz ampoule
(not closing, atmosphere is circulated), it is put into after quartz ampoule cooling and places into alloy and vacuumize sealing；
(4) quartz ampoule is put into dual temperature tube furnace, the heating-up temperature of powder heap is 860 DEG C (10-17Atm), alloy plus
Hot temperature is 1000 DEG C, heats 1h jointly, you can pure Al is formed on surface2O3Film, as shown in Figure 4.
Embodiment 4：
Surface sections of the sample of example 2 after 800 DEG C of oxidation 50h are as shown in figure 5, the mixed oxidization film prepared has well
Resistance to elevated temperatures.
Claims (4)
1. the standby Al of powder heap control oxygen compacting2O3And Cr2O3The method of film, it is characterised in that in vacuum environment, heat Fe-FeO
Powder heap is mixed, during mixing powder heap reaches balance, unnecessary oxygen can be absorbed or to discharge oxygen stable to obtain one
Oxygen pressure, oxygen pressure is controlled using Fe-FeO powder heaps, Al is prepared with addition element under low oxygen pressure2O3Film and Cr2O3Film, adjust
Section oxygen pressure can obtain pure Al2O3Film or Cr2O3The mixture of film or both, far less than preparing Al in an atmosphere2O3With
Cr2O3Al, Cr content of addition needed for film.
2. the standby Al of powder heap control oxygen compacting as claimed in claim 12O3And Cr2O3The method of film, it is characterised in that specific step
It is rapid as follows：
(1) after vacuum arc melting alloy in vacuum atmosphere homogenizing annealing 1 week；
(2) anneal after sample section, polished after grinding off surface scale, through alcohol and acetone cleaning remove surface impurity and
Greasy dirt；
(3) Fe-FeO powder heaps being put into quartz ampoule, depression will be burnt by then vacuumizing in the middle part of quartz ampoule, not closed in the middle part of quartz ampoule,
Atmosphere circulates while the alloy is separated with powder heap, is put into after quartz ampoule cooling and places into alloy and vacuumize sealing；
(4) heating-up temperature of Fe-FeO powder heaps is set in the range of 800~900 DEG C, Po2=10-17~10-20Atm, electric arc melting
The heating temperature range of alloy is 900~1000 DEG C, and insulation 1h can be obtained by complete pure Al2O3, pure Cr2O3Or both
Mixed layer.
3. the standby Al of powder heap control oxygen compacting as claimed in claim 1 or 22O3And Cr2O3The method of film, it is characterised in that institute
The mass ratio for stating Fe and FeO in Fe-FeO powder heaps is 1:1.
4. the standby Al of powder heap control oxygen compacting as claimed in claim 1 or 22O3And Cr2O3The method of film, it is characterised in that institute
It is ferrous alloy to state alloy, active containing Al, Cr in ferrous alloy and the oxide-film of fine and close protective can be formed on surface；Al
Content 3wt.%, Cr content 4-6wt.%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711002485.8A CN107858636A (en) | 2017-10-24 | 2017-10-24 | The standby Al of powder heap control oxygen compacting2O3And Cr2O3The method of film |
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|---|---|---|---|
| CN201711002485.8A CN107858636A (en) | 2017-10-24 | 2017-10-24 | The standby Al of powder heap control oxygen compacting2O3And Cr2O3The method of film |
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| CN107858636A true CN107858636A (en) | 2018-03-30 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111910148A (en) * | 2020-08-28 | 2020-11-10 | 浙江华达新型材料股份有限公司 | Method for forming compact oxide film on surface of Fe-Mn-Al alloy |
| CN113913713A (en) * | 2021-08-04 | 2022-01-11 | 常州大学 | Method for inhibiting Co ion release of Co-based biological material |
| CN114381684A (en) * | 2021-12-17 | 2022-04-22 | 常州大学 | A medicine prepared from Ca (OH)2Alloy surface treatment method for controlling water vapor pressure by mixing CaO and powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637050A (en) * | 2016-12-29 | 2017-05-10 | 常州大学 | Method for preparing antioxidant film under low oxygen pressure |
-
2017
- 2017-10-24 CN CN201711002485.8A patent/CN107858636A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637050A (en) * | 2016-12-29 | 2017-05-10 | 常州大学 | Method for preparing antioxidant film under low oxygen pressure |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111910148A (en) * | 2020-08-28 | 2020-11-10 | 浙江华达新型材料股份有限公司 | Method for forming compact oxide film on surface of Fe-Mn-Al alloy |
| CN113913713A (en) * | 2021-08-04 | 2022-01-11 | 常州大学 | Method for inhibiting Co ion release of Co-based biological material |
| CN113913713B (en) * | 2021-08-04 | 2023-01-17 | 常州大学 | Method for inhibiting Co ion release of Co-based biological material |
| CN114381684A (en) * | 2021-12-17 | 2022-04-22 | 常州大学 | A medicine prepared from Ca (OH)2Alloy surface treatment method for controlling water vapor pressure by mixing CaO and powder |
| CN114381684B (en) * | 2021-12-17 | 2024-04-02 | 常州大学 | Through Ca (OH) 2 Alloy surface treatment method for controlling water vapor pressure by mixing CaO powder |
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Application publication date: 20180330 |