CN102912290A - Preparation method of antioxidation Si-Zr-Y seepage coating on Nb-Ti-Si-base alloy surface - Google Patents
Preparation method of antioxidation Si-Zr-Y seepage coating on Nb-Ti-Si-base alloy surface Download PDFInfo
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- CN102912290A CN102912290A CN2012103272761A CN201210327276A CN102912290A CN 102912290 A CN102912290 A CN 102912290A CN 2012103272761 A CN2012103272761 A CN 2012103272761A CN 201210327276 A CN201210327276 A CN 201210327276A CN 102912290 A CN102912290 A CN 102912290A
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Abstract
The invention relates to a preparation method of an antioxidation Si-Zr-Y seepage coating on an Nb-Ti-Si-base alloy surface. The structure of the co-seepage coating is sequentially composed of a (Nb,X)Si2 outer layer, a (Ti,Nb)5Si4 transition layer and a Y-enriched (Nb,X)5Si3 inner layer from outside to inside. The preparation method comprises the following steps: accurately weighing a seepage agent, carrying out ball milling on the weighed seepage agent, putting the seepage agent into the crucible, burying a sample into the seepage agent, compacting, covering the crucible, sealing with silicasol and Al2O3, Y2O3 and ZrO2 powder, putting the crucible into a high-temperature high-vacuum controllable atmosphere diffusion seepage furnace, heating to 1000-1400 DEG C, and holding, wherein the holding time is controlled to prepare Si-Zr-Y co-seepage coatings with different thicknesses on the Nb-Ti-Si-base ultrahigh-temperature alloy surface.
Description
Technical field
The present invention relates to the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of a kind of Nb-Ti-Si base alloy surface, be exclusively used in preparation production and the application of the anti-oxidant Si-Zr-Y co-penetration layer of Nb-Ti-Si base alloy surface, belong to the metal surface properties modification technical field.
Background technology
The silica-based polynary ultrahigh temperature alloy of niobium has high-melting-point, low density and good hot strength; it is potential high about the 200 ℃ hot metal structured material of comparable nickel base superalloy use temperature; but its high-temperature oxidation resistance is relatively poor; although the high-temperature oxidation resistance through this alloy after multi-element alloyed has had significant raising; but still can't satisfy actual service requirements, thereby need to be at its surface preparation protective coating to improve its high-temperature oxidation resistance.Silicide coating density is low, fusing point is high, good thermal stability, is suitable for the high-temperature oxidation resistant protection of ultrahigh temperature alloy.But single silicide coating is owing to fragility own causes being prone to crackle in it, can produce larger internal stress in the coating during simultaneous oxidation, causes surface film oxide to peel off and loses protectiveness, therefore needs to add other element and carry out modification to it.Zr, Y isoreactivity element are improving coating compactness and with the bonding force of matrix, the aspects such as antistripping ability that fall low-alloyed rate of oxidation and improve oxide film unusual effect are being arranged, the people such as Zhai Jinkun adopt stuff paste melting to prepare the Si-Cr-Ti coating of Zr and Y modification at the C103 alloy surface, find the significantly crystal grain of refinement coating of Zr and Y element, improve density and the adhesivity of coating, 1400 ℃ of constant temperature oxidation experiments show, Zr, Y modification can significantly improve the high-temperature oxidation resistance of coating.
In recent years, the research that relates to the silica-based polynary ultrahigh temperature alloy of niobium surface high temperature coatings is also few, existing work mainly concentrates on the preparation of C103 alloy surface coating, and method also is mainly stuff paste melting, mainly have following problem: the coating structure of (1) stuff paste melting preparation is comparatively loose, hole and crackle can appear in coatingsurface and inside inevitably, and prepared coating high-temp antioxidant property is unsatisfactory; (2) because the atomic radius of Zr and Y is large and fusing point is higher, diffusion in alloy is difficulty comparatively, the active atomic that is respectively oozed simultaneously element also can influence each other in absorption and diffusion process, the more single silicide infiltration layer of the process of growth of co-penetration layer is more complicated, and conventional diffusion is oozed catalyzer (such as NH
4Cl, NH
4F and NaBr etc.) be difficult to prepare and ooze altogether respond well co-penetration layer.At present, the technology of preparing of the oxidation resistant Zr of the silica-based polynary ultrahigh temperature alloy surface high-temp of niobium, Y modified silicide infiltration layer and application thereof still belong to blank.Therefore the technology of preparing of research and the oxidation resistant Zr of the realization silica-based polynary ultrahigh temperature alloy surface high-temp of niobium, Y modified silicide infiltration layer is significant in the application of the industrial circles such as aerospace to the silica-based polynary ultrahigh temperature alloy of niobium.
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the present invention proposes the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of a kind of Nb-Ti-Si base alloy surface, can obtain bonding force good (metallurgical binding), evenly, fine and close Si-Zr-Y co-penetration layer, and have technique simple, easy to operate, with low cost, be easy to realize, the efficient advantages of higher, be suitable for producing and using.
Technical scheme
The preparation method of the anti-oxidant Si-Zr-Y infiltration layer of a kind of Nb-Ti-Si base alloy surface, it is characterized in that: infiltration layer is multilayered structure, from outside to inside successively by (Nb, X) Si
2Skin, (Ti, Nb)
5Si
4(Nb, the X) of transition layer and rich Y
5Si
3Internal layer; Described X represents element ti, Cr or Hf; Concrete preparation process is as follows:
The Si of step 1: by weight percentage: 10-25%, the Zr of 5-15%, the Y of 1-5%
2O
3, the NaF of 3-8%, all the other are Al
2O
3The preparation penetration enhancer;
Step 2: place ball mill to carry out the 4h ball milling penetration enhancer for preparing, drum's speed of rotation is 360 to turn/min;
Step 3: with the crucible of packing into of the penetration enhancer behind the ball milling, wish is made the material sample of infiltration layer again and imbedded in the penetration enhancer and compacting, the penetration enhancer thickness that specimen surface covers is not less than 10mm;
Step 4: crucible is added a cover and sealed, and sealing is placed on the diffusion of high temperature high vacuum controlled atmosphere and oozes in the stove; Described sealing material is silicon sol and Al
2O
3, Y
2O
3And ZrO
2The mixture of powder, ratio are to add 180g Al in every 100ml silicon sol
2O
3, 20g ZrO
2, 5gY
2O
3Powder;
Step 5: be evacuated down to 3.0 * 10
-2Beginning is heated with the temperature rise rate of 18 ℃/min behind the Pa, applying argon gas protection when being heated to 450 ℃, and then insulation 1-12h closed heating system and is chilled to room temperature with stove when temperature rose to 1000-1400 ℃;
Step 6: the material sample after diffusion oozed was ultrasonic cleaning 15 minutes, and then oven dry obtains anti-oxidant Si-Zr-Y infiltration layer at material sample.
80~1000#SiC liquid honing ultrasonic cleaning and drying up in dehydrated alcohol is adopted on the surface that described wish is made the material sample of infiltration layer.
When the material sample of a plurality of infiltration layers was arranged in the crucible in the described step 3, the distance between the adjacent, parallel material sample was not less than 15mm.
Described Si≤200 orders.
Described Zr≤200 orders.
Described Y
2O
3≤ 200 orders.
Described Al
2O
3≤ 200 orders.
It is analytical pure that described NaF adopts rank.
Beneficial effect
The preparation method of the anti-oxidant Si-Zr-Y infiltration layer of a kind of Nb-Ti-Si base alloy surface that the present invention proposes,
The invention solves the technical barrier of the anti-poor performance of Nb-Ti-Si Quito unit's ultrahigh temperature alloy high temperature, can obtain bonding force good (metallurgical binding), evenly, fine and close Si-Zr-Y co-penetration layer, and have technique simple, easy to operate, with low cost, be easy to realize, the efficient advantages of higher.Adopt 1250 ℃ of constant temperature oxidation experiments to detect, ooze altogether rear sample fine and close through 100h constant temperature oxidation rear oxidation film, rarely come off, show that co-penetration layer has excellent high-temperature oxidation resistance.
Processing method of the present invention can obtain bonding force good (metallurgical binding), even, fine and close Si-Zr-Y co-penetration layer, and have technique simple, easy to operate, with low cost, be easy to realize, the efficient advantages of higher, be suitable for producing and using.
Description of drawings
Fig. 1: technical process of the present invention;
Fig. 2: ooze altogether the macro morphology figure on co-penetration layer surface under the condition for the difference that adopts the present invention to obtain, wherein the temperature of oozing altogether of Fig. 2 (a) is 1000 ℃, and the time of oozing is 1h altogether, and the penetration enhancer component is 10Si-5Zr-1Y
2O
3-3NaF-81Al
2O
3(wt%); The temperature of oozing altogether of Fig. 2 (b) is 1250 ℃, and the time of oozing is 5h altogether, and the penetration enhancer component is 15Si-10Zr-3Y
2O
3-5NaF-67Al
2O
3(wt%); The temperature of oozing altogether of Fig. 2 (c) is 1400 ℃, and the time of oozing is 12h altogether, and the penetration enhancer component is 25Si-15Zr-5Y
2O
3-8NaF-47Al
2O
3(wt%).
Fig. 3: ooze altogether the microscopic appearance figure on co-penetration layer surface under the condition for the difference that adopts the present invention to obtain, wherein the temperature of oozing altogether of Fig. 3 (a) is 1000 ℃, and the time of oozing is 1h altogether, and the penetration enhancer component is 10Si-5Zr-1Y
2O
3-3NaF-81Al
2O
3(wt%); The temperature of oozing altogether of Fig. 3 (b) is 1250 ℃, and the time of oozing is 5h altogether, and the penetration enhancer component is 15Si-10Zr-3Y
2O
3-5NaF-67Al
2O
3(wt%); The temperature of oozing altogether of Fig. 3 (c) is 1400 ℃, and the time of oozing is 12h altogether, and the penetration enhancer component is 25Si-15Zr-5Y
2O
3-8NaF-47Al
2O
3(wt%);
Fig. 4: ooze altogether the microstructure figure in co-penetration layer cross section under the condition for the difference that adopts the present invention to obtain, wherein the temperature of oozing altogether of Fig. 4 (a) is 1000 ℃, and the time of oozing is 1h altogether, and the penetration enhancer component is 10Si-5Zr-1Y
2O
3-3NaF-81Al
2O
3(wt%); The temperature of oozing altogether of Fig. 4 (b) is 1250 ℃, and the time of oozing is 5h altogether, and the penetration enhancer component is 15Si-10Zr-3Y
2O
3-5NaF-67Al
2O
3(wt%); The temperature of oozing altogether of Fig. 4 (c) is 1400 ℃, and the time of oozing is 12h altogether, and the penetration enhancer component is 25Si-15Zr-5Y
2O
3-8NaF-47Al
2O
3(wt%);
Fig. 5: the element that oozes altogether co-penetration layer cross section under the condition for the difference that adopts the present invention to obtain distributes, and wherein the temperature of oozing altogether of Fig. 5 (a) is 1000 ℃, and the time of oozing is 1h altogether, and the penetration enhancer component is 10Si-5Zr-1Y
2O
3-3NaF-81Al
2O
3(wt%); The temperature of oozing altogether of Fig. 5 (b) is 1250 ℃, and the time of oozing is 5h altogether, and the penetration enhancer component is 15Si-10Zr-3Y
2O
3-5NaF-67Al
2O
3(wt%); The temperature of oozing altogether of Fig. 5 (c) is 1400 ℃, and the time of oozing is 12h altogether, and the penetration enhancer component is 25Si-15Zr-5Y
2O
3-8NaF-47Al
2O
3(wt%);
Fig. 6: be the macro morphology of sample behind 1250 ℃ of constant temperature oxidation 100h after oozing altogether through 1250 ℃/5h.
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Embodiment 1
1. prepare sample: sample is placed on ultrasonic cleaning in the alcohol through each face of 1000# sand papering, dries up for subsequent use; 2. prepare penetration enhancer: accurately take by weighing according to quantity penetration enhancer, the proportioning of penetration enhancer is by weight percentage: 200 purpose silicon, content is 10%, 200 purpose zirconiums, content are 5%, 200 purpose yttrium oxide, content is 1%, Sodium Fluoride is analytical pure (99%), content 3%, and all the other are for being 200 purpose aluminium sesquioxides; 3. ball milling: the penetration enhancer for preparing is placed satellite gear ball mill spheroidal graphite 4h, its abundant refinement is mixed; 4. fill sample: with the crucible of packing into of the penetration enhancer behind the ball milling, and imbed in the penetration enhancer sample and compacting, the distance between the adjacent, parallel sample is not less than 15mm, and the penetration enhancer thickness that specimen surface covers is not less than 10mm; 5. sealing: the crucible that sample will be housed is added a cover and with silicon sol and Al
2O
3, Y
2O
3And ZrO
2Powder-tight is placed on the diffusion of high temperature high vacuum controlled atmosphere and oozes in the stove; 6. diffusion is oozed: system is evacuated down to 3.0 * 10
-2Beginning is heated with the temperature rise rate of 18 ℃/min behind the Pa, applying argon gas protection when being heated to 450 ℃, and then insulation 1h closed heating system when temperature rose to 1000 ℃, and sample is chilled to room temperature with stove; 7. cleaning, drying: the sample after will oozing altogether uses alcohol ultrasonic irrigation 15min, dries again, finishes.
Embodiment 2
1. prepare sample: sample is placed on ultrasonic cleaning in the alcohol through each face of 1000# sand papering, dries up for subsequent use; 2. prepare penetration enhancer: accurately take by weighing according to quantity penetration enhancer, the proportioning of penetration enhancer is by weight percentage: 200 purpose silicon, content is 15%, 200 purpose zirconiums, content are 10%, 200 purpose yttrium oxide, content is 3%, Sodium Fluoride is analytical pure (99%), content 5%, and all the other are for being 200 purpose aluminium sesquioxides; 3. ball milling: the penetration enhancer for preparing is placed satellite gear ball mill spheroidal graphite 4h, its abundant refinement is mixed; 4. fill sample: with the crucible of packing into of the penetration enhancer behind the ball milling, and imbed in the penetration enhancer sample and compacting, the distance between the adjacent, parallel sample is not less than 15mm, and the penetration enhancer thickness that specimen surface covers is not less than 10mm; 5. sealing: the crucible that sample will be housed is added a cover and with silicon sol and Al
2O
3, Y
2O
3And ZrO
2Powder-tight is placed on the diffusion of high temperature high vacuum controlled atmosphere and oozes in the stove; 6. diffusion is oozed: system is evacuated down to 3.0 * 10
-2Beginning is heated with the temperature rise rate of 18 ℃/min behind the Pa, applying argon gas protection when being heated to 450 ℃, and then insulation 5h closed heating system when temperature rose to 1250 ℃, and sample is chilled to room temperature with stove; 7. cleaning, drying: the sample after will oozing altogether uses alcohol ultrasonic irrigation 15min, dries again, finishes.
Embodiment 3:
1. prepare sample: sample is placed on ultrasonic cleaning in the alcohol through each face of 1000# sand papering, dries up for subsequent use; 2. prepare penetration enhancer: accurately take by weighing according to quantity penetration enhancer, the proportioning of penetration enhancer is by weight percentage: 200 purpose silicon, content is 25%, 200 purpose zirconiums, content are 15%, 200 purpose yttrium oxide, content is 5%, Sodium Fluoride is analytical pure (99%), content 8%, and all the other are for being 200 purpose aluminium sesquioxides; 3. ball milling: the penetration enhancer for preparing is placed satellite gear ball mill spheroidal graphite 4h, its abundant refinement is mixed; 4. fill sample: with the crucible of packing into of the penetration enhancer behind the ball milling, and imbed in the penetration enhancer sample and compacting, the distance between the adjacent, parallel sample is not less than 15mm, and the penetration enhancer thickness that specimen surface covers is not less than 10mm; 5. sealing: the crucible that sample will be housed is added a cover and with silicon sol and Al
2O
3, Y
2O
3And ZrO
2Powder-tight is placed on the diffusion of high temperature high vacuum controlled atmosphere and oozes in the stove; 6. diffusion is oozed: system is evacuated down to 3.0 * 10
-2Beginning is heated with the temperature rise rate of 18 ℃/min behind the Pa, applying argon gas protection when being heated to 450 ℃, and then insulation 12h closed heating system when temperature rose to 1400 ℃, and sample is chilled to room temperature with stove; 7. cleaning, drying: the sample after will oozing altogether uses alcohol ultrasonic irrigation 15min, dries again, finishes.
Claims (8)
1. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of Nb-Ti-Si base alloy surface, it is characterized in that: infiltration layer is multilayered structure, from outside to inside successively by (Nb, X) Si
2Skin, (Ti, Nb)
5Si
4(Nb, the X) of transition layer and rich Y
5Si
3Internal layer; Described X represents element ti, Cr or Hf; Concrete preparation process is as follows:
The Si of step 1: by weight percentage: 10-25%, the Zr of 5-15%, the Y of 1-5%
2O
3, the NaF of 3-8%, all the other are Al
2O
3The preparation penetration enhancer;
Step 2: place ball mill to carry out the 4h ball milling penetration enhancer for preparing, drum's speed of rotation is 360 to turn/min;
Step 3: with the crucible of packing into of the penetration enhancer behind the ball milling, wish is made the material sample of infiltration layer again and imbedded in the penetration enhancer and compacting, the penetration enhancer thickness that specimen surface covers is not less than 10mm;
Step 4: crucible is added a cover and sealed, and sealing is placed on the diffusion of high temperature high vacuum controlled atmosphere and oozes in the stove; Described sealing material is silicon sol and Al
2O
3, Y
2O
3And ZrO
2The mixture of powder, ratio are to add 180g Al in every 100ml silicon sol
2O
3, 20g ZrO
2, 5gY
2O
3Powder;
Step 5: be evacuated down to 3.0 * 10
-2Beginning is heated with the temperature rise rate of 18 ℃/min behind the Pa, applying argon gas protection when being heated to 450 ℃, and then insulation 1-12h closed heating system and is chilled to room temperature with stove when temperature rose to 1000-1400 ℃;
Step 6: the material sample after diffusion oozed was ultrasonic cleaning 15 minutes, and then oven dry obtains anti-oxidant Si-Zr-Y infiltration layer at material sample.
2. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of described Nb-Ti-Si base alloy surface according to claim 1 is characterized in that: 80~1000#SiC liquid honing ultrasonic cleaning and drying up in dehydrated alcohol is adopted on the surface that described wish is made the material sample of infiltration layer.
3. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of described Nb-Ti-Si base alloy surface according to claim 1, it is characterized in that: when the material sample of a plurality of infiltration layers was arranged in the crucible in the described step 3, the distance between the adjacent, parallel material sample was not less than 15mm.
4. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of described Nb-Ti-Si base alloy surface according to claim 1 is characterized in that: described Si≤200 orders.
5. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of described Nb-Ti-Si base alloy surface according to claim 1 is characterized in that: described Zr≤200 orders.
6. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of described Nb-Ti-Si base alloy surface according to claim 1 is characterized in that: described Y
2O
3≤ 200 orders.
7. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of described Nb-Ti-Si base alloy surface according to claim 1 is characterized in that: described Al
2O
3≤ 200 orders.
8. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of described Nb-Ti-Si base alloy surface according to claim 1, it is characterized in that: it is analytical pure that described NaF adopts rank.
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Cited By (7)
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CN103949590A (en) * | 2014-05-12 | 2014-07-30 | 西北工业大学 | Preparation method of oxide doped and modified Y2O3+YSZ high-temperature-resisting shell |
CN103993259A (en) * | 2014-04-25 | 2014-08-20 | 西北工业大学 | Two-step preparation method for Y and Al modified silicide infiltrated layer on surface of Nb-Si-based alloy |
CN104911537A (en) * | 2015-06-09 | 2015-09-16 | 西北工业大学 | Nb-Ti-Si-base alloy surface B-Y modified silicide coating and preparation method thereof |
CN106435460A (en) * | 2016-10-18 | 2017-02-22 | 中国矿业大学 | Niobium alloy surface high-temperature abrasion resisting coating and preparation method thereof |
CN107267915A (en) * | 2017-06-24 | 2017-10-20 | 北方民族大学 | A kind of penetration enhancer and method for preparing tantalum and tantalum alloy surface Si B Y coatings |
CN110863172A (en) * | 2019-11-16 | 2020-03-06 | 北方民族大学 | Cr-Si-Zr-B permeating agent and application method thereof on tantalum and tantalum alloy surface |
CN112191802A (en) * | 2020-09-23 | 2021-01-08 | 西北工业大学 | Preparation method of Nb-Si-based ultrahigh-temperature alloy directional solidification blade simulation piece |
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CN103993259A (en) * | 2014-04-25 | 2014-08-20 | 西北工业大学 | Two-step preparation method for Y and Al modified silicide infiltrated layer on surface of Nb-Si-based alloy |
CN103949590A (en) * | 2014-05-12 | 2014-07-30 | 西北工业大学 | Preparation method of oxide doped and modified Y2O3+YSZ high-temperature-resisting shell |
CN104911537A (en) * | 2015-06-09 | 2015-09-16 | 西北工业大学 | Nb-Ti-Si-base alloy surface B-Y modified silicide coating and preparation method thereof |
CN104911537B (en) * | 2015-06-09 | 2017-10-13 | 西北工业大学 | Nb Ti Si based alloys surface B Y modified silicides coatings and preparation method |
CN106435460A (en) * | 2016-10-18 | 2017-02-22 | 中国矿业大学 | Niobium alloy surface high-temperature abrasion resisting coating and preparation method thereof |
CN107267915A (en) * | 2017-06-24 | 2017-10-20 | 北方民族大学 | A kind of penetration enhancer and method for preparing tantalum and tantalum alloy surface Si B Y coatings |
CN110863172A (en) * | 2019-11-16 | 2020-03-06 | 北方民族大学 | Cr-Si-Zr-B permeating agent and application method thereof on tantalum and tantalum alloy surface |
CN112191802A (en) * | 2020-09-23 | 2021-01-08 | 西北工业大学 | Preparation method of Nb-Si-based ultrahigh-temperature alloy directional solidification blade simulation piece |
CN112191802B (en) * | 2020-09-23 | 2022-04-12 | 西北工业大学 | Preparation method of Nb-Si-based ultrahigh-temperature alloy directional solidification blade simulation piece |
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