CN1818124A - High-temperature antioxidant chiomium modified sillicide coating and preparation thereof - Google Patents

High-temperature antioxidant chiomium modified sillicide coating and preparation thereof Download PDF

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CN1818124A
CN1818124A CNA2006100650594A CN200610065059A CN1818124A CN 1818124 A CN1818124 A CN 1818124A CN A2006100650594 A CNA2006100650594 A CN A2006100650594A CN 200610065059 A CN200610065059 A CN 200610065059A CN 1818124 A CN1818124 A CN 1818124A
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coating
layer
matrix alloy
salt
phase
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CN100462471C (en
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李树索
周春根
王永平
韩雅芳
宫声凯
徐惠彬
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Beihang University
Beijing University of Aeronautics and Astronautics
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Beihang University
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Abstract

The invention opened an anti-high temperature oxidation silicide coating modified by the chrome. It has two layers, the inner layer is NbxSi1-x and the atomic mass of the x is 28-35; the outer layer is the two-phase chrome-siliconized layer, the first phase is Cr56-60Si35-41Al2-5 and the second phase is Cr71-76Si21-27Nb1-5. The coasting is to form the NbSi2 inner layer by the molten salt method then to form the two phase chrome-siliconized layer out of the alloy. The alloy of Nb35-50Ti22-26Si14-18Cr4-8Al4-6Hf2-8 is oxidized for 100h in the 1250 DEG C, the weight is improved by 3.5-4.5mg/cm2 and the oxidation resistance has improved by 80 times.

Description

The chromium modified silicide coating of resistance to high temperature oxidation and the preparation method of coating thereof
Technical field
The present invention relates to a kind of silicide coating material of resistance to high temperature oxidation, more particularly say, be meant a kind of chromium modified silicide coating of the Nb-Ti-Si-Cr-Al-Hf of being applicable to matrix alloy resistance to high temperature oxidation, and the preparation method of chromium modified silicide coating.
Background technology
Nb-Ti-Si-Cr-Al-Hf (Nb base altogether solution) advantages such as alloy has the fusing point height, density is low and hot strength and creep-resistant property be good, it is one of following high-performance gas turbine engine ideal candidate material, but the subject matter that this material exists at present is relatively poor at the antioxidant property of hot environment, and the oxidation weight gain behind 20～80h under 1250 ℃ of atmospheric environments of high temperature is 37.5～129.7mg/cm 2(oxidation weight gain curve is referring to shown in Figure 2).Adopt alloyage process to prepare the Nb-Ti-Si-Cr-Al-Hf alloy,, significant limitation is arranged though the antioxidant property of Nb-Ti-Si-Cr-Al-Hf alloy is made moderate progress.In order to improve the high-temperature oxidation resistance of Nb-Ti-Si-Cr-Al-Hf alloy, the inventor proposes a kind of molten-salt growth method that adopts earlier and forms certain thickness NbSi on the matrix alloy surface 2Coating adopts the pack cementation method having NbSi then 2Form the oxidation susceptibility that the chromsiliconizing layer overcomes matrix alloy on the coating of material alloy.
Summary of the invention
One of purpose of the present invention provides the oxidation resistant chromium modified silicide coated material of a kind of Nb-Ti-Si-Cr-Al-Hf of raising matrix alloy surface under hot conditions.
Another object of the present invention is the preparation technology who proposes a kind of chromium modified silicide coated material of the Nb-Ti-Si-Cr-Al-Hf of raising matrix alloy high-temperature oxidation resistant.
The chromium modified silicide coating of a kind of resistance to high temperature oxidation of the present invention, its chromium modified silicide coating are to prepare on Nb-Ti-Si-Cr-Al-Hf matrix alloy surface, and are bilayer structure, and the composition of its coating internal layer is Nb XSi 1～X, the atom consumption of X is 28～35, and its coating skin is a two-phase chromsiliconizing layer, and the composition of the first phase chromsiliconizing layer is Cr 56～60Si 35～41Al 2～5, the composition of the second phase chromsiliconizing layer is Cr 71～76Si 21～27Nb 1～5, the chemical ingredients of described Nb-Ti-Si-Cr-Al-Hf matrix alloy is the Nb of 38～50wt%, the Ti of 22～26wt%, and the Si of 14～18wt%, the Cr of 4～8wt%, the Al of 4～6wt% and the Hf of 2～8wt% form.
The chromium modified silicide coating of described resistance to high temperature oxidation, the composition of coating internal layer is Nb 67Si 33, the composition of the outer field first phase chromsiliconizing layer of coating is Cr 58Si 39Al 3, the composition of the second phase chromsiliconizing layer is Cr 74Si 24Nb 2
The preparation method of the chromium modified silicide coating of described resistance to high temperature oxidation has the following step:
The first step: adopt molten-salt growth method at matrix alloy surface preparation coating internal layer
Matrix alloy is imbedded in the fused salt in the crucible, and described crucible is put into process furnace, be heated to 800 ℃～1000 ℃, and after being incubated 5～9 hours, furnace cooling prepares at Nb promptly 38～50Ti 22～26Si 14～18Cr 4～8Al 4～6Hf 2～8Coating internal layer on the matrix alloy;
Described fused salt is made up of 180～240 purpose silicon Si powder and 180～240 purpose salt, and the consumption of described silicon Si powder accounts for 1/10～1/8 of described salt consumption, and described salt is NaCl+KCl+NaF+Na 2SiF 6The mixing salt of forming, described mixing salt composition is the Na of 30～36wt%NaCl, 30～36wt%KCl, 20～22wt%NaF and surplus 2SiF 6
Second step: adopt the pack cementation legal system to be equipped with the coating skin
Will the matrix alloy after the first step is handled imbed in the chromising modified coating penetration enhancer in the crucible, and described crucible placed in the high temperature resistance furnace, feed the shielding gas argon gas of 0.5～3.0L/min, heating resistor stove to 1100 ℃～1500 ℃, and after being incubated 1.5～3 hours, furnace cooling promptly prepares the chromium modified silicide coating on the coating internal layer;
Described chromising modified coating penetration enhancer is by 180～240 purposes, 4.5～6.5wt%Si, 180～240 purposes, 20～30wt%Cr, 80～120 purposes, 2～4wt%NH 4Cl and surplus 80～120 purpose Al 2O 3Form.
The advantage of chromium modified silicide coated material of the present invention is: because chromium modified silicide coating is a bilayer structure, coating forms the SiO of continuous densification under hot environment 2Stoped matrix alloy oxidized.Its silicide layer (being coating internal layer 2) is single-phase NbSi 2Very crisp, a lot of crackles appear in its surface, make the surface smoothing flawless of matrix alloy by embedding chromising modified coating penetration enhancer on silicide layer.Preparation has the Nb of chromium modified silicide coating 38～50Ti 22～26Si 14～18Cr 4～8Al 4～6Hf 2～8After 100 hours, its oxidation weight gain is 2.5～4.5mg/cm to matrix alloy 1250 ℃ of constant temperature oxidations 2, improving on the antioxidant property about 15～80 times than the matrix alloy of handling without coating.
The advantage that the present invention prepares chromium modified silicide coated material is: adopt molten-salt growth method+compound preparation technology of pack cementation method to prepare certain thickness chromium modified silicide coating on the matrix alloy surface, its surface smoothing flawless, the coating on matrix alloy surface can form the SiO of continuous densification during high temperature oxidation 2Stop the diffusion of oxygen effectively, improved Nb effectively to matrix alloy inside 38～50Ti 22～26Si 14～18Cr 4～8Al 4～6Hf 2～8The performance of matrix alloy high-temperature oxidation resistant.
Description of drawings
Fig. 1 is the structural representation of chromium modified silicide coating of the present invention.
Fig. 2 is the Nb base oxidation weight gain curve of solution alloy under 1250 ℃ of atmospheric environments altogether.
Fig. 3 is the Nb with chromium modified silicide coating of the present invention 40Ti 24Si 16Cr 6Al 6Hf 8The oxidation weight gain curve of matrix alloy under 1250 ℃ of atmospheric environments.
Fig. 4 is the sem photograph of the coating internal layer for preparing of the present invention.
Fig. 5 is the outer field sem photograph of coating that the present invention prepares.
Among the figure: 1. matrix alloy 2. coating internal layers 3. coating skins
Embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing.
See also shown in Figure 1, the present invention is a kind of chromium modified silicide coating that adopts molten-salt growth method+compound preparation resistance to high temperature oxidation of pack cementation method on Nb-Ti-Si-Cr-Al-Hf matrix alloy 1 surface, described chromium modified silicide coating is a bilayer structure, and the composition of its coating internal layer 2 is Nb XSi 1～X, the atom consumption of X is 28～35; Its coating outer 3 is a two-phase chromsiliconizing layer, and the composition of the first phase chromsiliconizing layer is Cr 56～60Si 35～41Al 2～5, the composition of the second phase chromsiliconizing layer is Cr 71～76Si 21～27Nb 1～5
The present invention is a kind of in the Nb-Ti-Si-Cr-Al-Hf matrix alloy 1 surperficial chromium modified silicide coating that adopts molten-salt growth method to add the compound preparation resistance to high temperature oxidation of pack cementation method, and its preparation technology is:
The first step: adopt molten-salt growth method at matrix alloy 1 surface preparation coating internal layer 2 (being silicide coating)
Matrix alloy 1 is imbedded in the fused salt in the crucible, and described crucible is put into process furnace (the model SK-6-12 tubular electric resistance that Beijing Electric Stove Factory produces); The following insulation of temperature condition that is heated to 800 ℃～1000 ℃ is after 5～9 hours, and furnace cooling promptly prepares at Nb 38～50Ti 22～26Si 14～18Cr 4～8Al 4～6Hf 2～8Coating internal layer 2 on the matrix alloy 1;
Described fused salt is made up of 180～240 purpose silicon Si powder and 180～240 purpose salt, and the consumption of described silicon Si powder accounts for 1/10～1/8 of described salt consumption, and described salt is NaCl+KCl+NaF+Na 2SiF 6The mixing salt of forming, described mixing salt composition is the Na of 30～36wt%NaCl, 30～36wt%KCl, 20～22wt%NaF and surplus 2SiF 6
Second step: adopt the pack cementation legal system to be equipped with coating skin 3 (being the chromium modified coating)
Will the matrix alloy 1 after the first step is handled imbed in the chromising modified coating penetration enhancer in the crucible, and described crucible is placed high temperature resistance furnace (the model SK that Beijing Electric Stove Factory produces 2-2.5-13S type tube furnace) in; Feed the shielding gas argon gas of 0.5～3.0L/min, insulation is after 1.5～3 hours down for the temperature condition of heating resistor stove to 1100 ℃～1500 ℃, and furnace cooling promptly prepares the chromium modified silicide coating on coating internal layer 2;
Described chromising modified coating penetration enhancer is by 180～240 purposes, 4.5～6.5wt%Si, 180～240 purposes, 20～30wt%Cr, 80～120 purposes, 2～4wt%NH 4Cl and surplus 80～120 purpose Al 2O 3Form.
After 100 hours, its oxidation weight gain is 2.5～4.5mg/cm to the Nb-Ti-Si-Cr-Al-Hf matrix alloy of the chromium modified silicide coating with high-temperature oxidation resistant that will prepare through above-mentioned molten-salt growth method+pack cementation method recombining process 1250 ℃ of constant temperature oxidations 2, make body material obtain good protection.The TG328A type optical readings analytical balance that adopts Hunan instrument balance equipment factory to produce to the oxidation weighing of Nb-Ti-Si-Cr-Al-Hf matrix alloy with chromium modified silicide coating.
Chromium modified silicide coating of the present invention, the main component of its coating internal layer is single-phase NbSi 2Very crisp, a lot of crackles (seeing also shown in Figure 4) appear in its surface, make the surface smoothing flawless (seeing also shown in Figure 5) of matrix alloy by embedding chromising modified coating penetration enhancer on silicide layer.
Improved the high-temperature oxidation resistance of Nb-Ti-Si-Cr-Al-Hf matrix alloy effectively by molten-salt growth method of the present invention+compound preparation technology of pack cementation method, enlarged the use range of this alloy material, simultaneously this material has been achieved as the material of gas turbine engine.
Embodiment 1:At matrix alloy Nb 40Ti 24Si 16Cr 6Al 6Hf 8Last preparation chromium modified silicide coating
Raw materials used, equipment and processing parameter see the following form:
Molten-salt growth method The pack cementation method
Raw material Si NaCl KCl NaF Na 2SiF 6 Si Cr NH 4Cl Al 2O 3
50g 180g 150g 100g 70g 30g 100g 18g 600g
The coating internal layer Nb 67Si 33
The first phase chromsiliconizing layer Cr 58Si 39Al 3
The second phase chromsiliconizing layer Cr 74Si 24Nb 2
Equipment Process furnace Resistance furnace
Shielding gas Do not have Argon gas Preceding 10min 3.0L/min
0.7L/min behind the 10min
Heating temperature 1000℃ 1200℃
Reaction times 6 hours 2 hours
It is stand-by at first to take by weighing desired raw material at experimentation:
Weighing fused salt: the Si and the 500g 200 order salt of 50g 200 order purity 99.9% are mixed, put into crucible.Wherein, the amount of taking by weighing of salt is 180g NaCl, 150g KCl, 100g NaF and 70g Na 2SiF 6
Weighing chromising modified coating penetration enhancer: with Si, the Cr of 100g 200 order purity 99.9%, the NH of 18g 120 order purity 99.9% of 30g 200 order purity 99.9% 4The Al of Cl and 600g 120 order purity 99.9% 2O 3Mix, put into crucible.
Preparation coating internal layer 2 in the process furnace:
The parameter that goes out according to last tabular, 1000 ℃ of the temperature of reaction by the control process furnace, 6 hours reaction times made Nb 67Si 33The coating internal layer.
Preparation coating skin 3 in the resistance furnace:
The parameter that goes out according to last tabular, 1200 ℃ of the temperature of reaction by the controlling resistance stove, 2 hours reaction times, simultaneously the flow velocity of shielding gas argon gas is controlled, make biphase coating skin, i.e. Cr 58Si 39Al 3First phase chromsiliconizing layer and the Cr 74Si 24Nb 2The second phase chromsiliconizing layer.
With above-mentioned prepare have a coating internal layer Nb 67Si 33With coating skin (the first chromsiliconizing layer Cr mutually 58Si 39Al 3+ the second phase chromsiliconizing layer Cr 74Si 24Nb 2) Nb 40Ti 24Si 16Cr 6Al 6Hf 8Matrix alloy carries out antioxidant property test, its 1250 ℃ of constant temperature oxidations after 80 hours its oxidation weight gain be 1.65mg/cm 2(seeing also shown in Figure 3), and without the Nb of the inventive method modification 40Ti 24Si 16Cr 6Al 6Hf 8Matrix alloy 1250 ℃ of constant temperature oxidations after 80 hours its oxidation weight gain be 139mg/cm 2(seeing also shown in Figure 2), the Nb with chromium modified silicide coating 40Ti 24Si 16Cr 6Al 6Hf 8The high-temperature oxidation resistance of matrix alloy has improved 84 times.
Embodiment 2:At matrix alloy Nb 46Ti 24Si 16Cr 6Al 6Hf 2Last preparation chromium modified silicide coating
Raw materials used, equipment and processing parameter see the following form:
Molten-salt growth method The pack cementation method
Raw material Si NaCl KCl NaF Na 2SiF 6 Si Cr NH 4Cl Al 2O 3
50g 180g 150g 100g 70g 30g 100g 18g 600g
The coating internal layer Nb 67Si 33
The first phase chromsiliconizing layer Cr 58Si 39Al 3
The second phase chromsiliconizing layer Cr 74Si 24Nb 2
Equipment Process furnace Resistance furnace
Shielding gas Do not have Argon gas Preceding 10min 3.0L/min
0.7L/min behind the 10min
Heating temperature 900℃ 1300℃
Reaction times 8 hours 1.5 hour
Preparation process is identical with embodiment 1, and difference is the time to the setting and the reaction of humidity.
Preparation there is coating internal layer Nb 67Si 33With coating skin (the first chromsiliconizing layer Cr mutually 58Si 39Al 3+ the second phase chromsiliconizing layer Cr 74Si 24Nb 2) Nb 40Ti 24Si 16Cr 6Al 6Hf 2Matrix alloy carries out antioxidant property test, its 1250 ℃ of constant temperature oxidations after 100 hours its oxidation weight gain only be 3.5mg/cm 2, and without the Nb of the inventive method modification 40Ti 24Si 16Cr 6Al 6Hf 2Matrix alloy 1250 ℃ of constant temperature oxidations after 100 hours its oxidation weight gain be 189mg/cm 2, Nb with chromium modified silicide coating 40Ti 24Si 16Cr 6Al 6Hf 2The high-temperature oxidation resistance of matrix alloy has improved 54 times.

Claims (5)

1, a kind of chromium modified silicide coating of resistance to high temperature oxidation is characterized in that: described chromium modified silicide coating is to prepare on Nb-Ti-Si-Cr-Al-Hf matrix alloy (1) surface, and is bilayer structure, and the composition of its coating internal layer (2) is Nb XSi 1～X, the atom consumption of X is 28～35, and its coating skin (3) is a two-phase chromsiliconizing layer, and the composition of the first phase chromsiliconizing layer is Cr 56～60Si 35～41Al 2～5, the composition of the second phase chromsiliconizing layer is Cr 71～76Si 21～27Nb 1～5, the chemical ingredients of described Nb-Ti-Si-Cr-Al-Hf matrix alloy (1) is the Nb of 38～50wt%, the Ti of 22～26wt%, and the Si of 14～18wt%, the Cr of 4～8wt%, the Al of 4～6wt% and the Hf of 2～8wt% form.
2, the chromium modified silicide coating of resistance to high temperature oxidation according to claim 1, it is characterized in that: the composition of described coating internal layer (2) is Nb 67Si 33
3, the chromium modified silicide coating of resistance to high temperature oxidation according to claim 1 is characterized in that: the composition of the first phase chromsiliconizing layer of described coating skin (3) is Cr 58Si 39Al 3, the composition of the second phase chrome-silicon codoping layer is Cr 74Si 24Nb 2
4, a kind of method for preparing the chromium modified silicide coating of resistance to high temperature oxidation as claimed in claim 1 is characterized in that the following step is arranged:
The first step: adopt molten-salt growth method at matrix alloy (1) surface preparation coating internal layer (2)
Matrix alloy (1) is imbedded in the fused salt in the crucible, and described crucible is put into process furnace, be heated to 800 ℃～1000 ℃, and after being incubated 5～9 hours, furnace cooling prepares at Nb promptly 38～50Ti 22～26Si 14～18Cr 4～8Al 4～6Hf 2～8Coating internal layer (2) on the matrix alloy (1);
Described fused salt is made up of 180～240 purpose silicon Si powder and 180～240 purpose salt, and the consumption of described silicon Si powder accounts for 1/10～1/8 of described salt consumption, and described salt is NaCl+KCl+NaF+Na 2SiF 6The mixing salt of forming, described mixing salt composition is the Na of 30～36wt%NaCl, 30～36wt%KCl, 20～22wt%NaF and surplus 2SiF 6
Second step: adopt the pack cementation legal system to be equipped with coating skin (3)
Will the matrix alloy (1) after the first step is handled imbed in the chromising modified coating penetration enhancer in the crucible, and described crucible placed in the high temperature resistance furnace, feed the shielding gas argon gas of 0.5～3.0L/min, heating resistor stove to 1100 ℃～1500 ℃, and after being incubated 1.5～3 hours, furnace cooling promptly prepares the chromium modified silicide coating on coating internal layer (2);
Described chromising modified coating penetration enhancer is by 180～240 purposes, 4.5～6.5wt%Si, 180～240 purposes, 20～30wt%Cr, 80～120 purposes, 2～4wt%NH 4Cl and surplus 80～120 purpose Al 2O 3Form.
5, the method for the chromium modified silicide coating of preparation resistance to high temperature oxidation according to claim 4 is characterized in that: the Nb of preparation 38～50Ti 22～26Si 14～18Cr 4～8Al 4～6Hf 2～8Matrix alloy 1250 ℃ of constant temperature oxidations after 100 hours its oxidation weight gain be 2.5～4.5mg/cm 2
CNB2006100650594A 2006-03-17 2006-03-17 High-temperature antioxidant chiomium modified sillicide coating and preparation thereof Expired - Fee Related CN100462471C (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102030544A (en) * 2010-10-09 2011-04-27 北京航空航天大学 Preparation method of high temperature-resistant, radiation-insulated, heat-conducting and microwave-permeable inorganic coating
CN105290389B (en) * 2015-11-13 2018-02-06 航天材料及工艺研究所 A kind of micro-satellite cluster thrust chamber slurry and its preparation method and application

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT208675B (en) * 1959-02-06 1960-04-25 Plansee Metallwerk Process for the production of protective layers on, in particular, refractory metals
GB939609A (en) * 1961-01-30 1963-10-16 North American Aviation Inc Diffusion coating method for metals and alloys

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102030544A (en) * 2010-10-09 2011-04-27 北京航空航天大学 Preparation method of high temperature-resistant, radiation-insulated, heat-conducting and microwave-permeable inorganic coating
CN105290389B (en) * 2015-11-13 2018-02-06 航天材料及工艺研究所 A kind of micro-satellite cluster thrust chamber slurry and its preparation method and application

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