CN102912290B - 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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- CN102912290B CN102912290B CN201210327276.1A CN201210327276A CN102912290B CN 102912290 B CN102912290 B CN 102912290B CN 201210327276 A CN201210327276 A CN 201210327276A CN 102912290 B CN102912290 B CN 102912290B
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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, the preparation that is exclusively used in the anti-oxidant Si-Zr-Y co-penetration layer of Nb-Ti-Si base alloy surface is produced and application, belongs to 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 the hot metal structured material of potential high 200 DEG C of left and right of comparable nickel base superalloy use temperature; but its high-temperature oxidation resistance is poor; although the high-temperature oxidation resistance of this alloy has had significant raising after multi-element alloyed; but still cannot meet actual service requirements, thereby need to prepare on its surface 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, because fragility own causes being prone to crackle in it, can produce larger internal stress in coating when simultaneous oxidation, causes surface film oxide to peel off and loses protectiveness, therefore needs to add other element it is carried out to modification.Zr, Y isoreactivity element are improving coating compactness and are having unusual effect with the bonding force of matrix, the aspect such as antistripping ability that falls low-alloyed rate of oxidation and improve oxide film, the people such as Zhai Jinkun adopt stuff paste melting to prepare the Si-Cr-Ti coating of Zr and Y modification at C103 alloy surface, find the significantly crystal grain of refinement coating of Zr and Y element, improve density and the adhesivity of coating, 1400 DEG C 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 is also mainly stuff paste melting, mainly there is following problem: coating structure prepared by (1) stuff paste melting is comparatively loose, can inevitably there is hole and crackle in coatingsurface and inside, 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 element also can influence each other simultaneously in absorption and diffusion process, the more single silicide infiltration layer of process of growth of co-penetration layer is more complicated, and conventional diffusion is oozed catalyzer (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 studying and realize the oxidation resistant Zr of the 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 solving
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, efficiency advantages of higher, be suitable for produce and application.
Technical scheme
A preparation method for the anti-oxidant Si-Zr-Y infiltration layer of Nb-Ti-Si base alloy surface, 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
3preparation penetration enhancer;
Step 2: the penetration enhancer preparing is placed in to ball mill and carries out 4h ball milling, drum's speed of rotation is 360 turn/min;
Step 3: pack the penetration enhancer after ball milling into crucible, then the material sample that wish is made infiltration layer is imbedded in 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 stove; Described sealing material is silicon sol and Al
2o
3, Y
2o
3and ZrO
2the mixture of powder, ratio is 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
-2after Pa, start to heat with the temperature rise rate of 18 DEG C/min, applying argon gas protection while being heated to 450 DEG C, temperature is incubated 1-12h while rising to 1000-1400 DEG C, then close heating system and be chilled to room temperature with stove;
Step 6: the material sample after diffusion is oozed, ultrasonic cleaning 15 minutes, is then dried, and obtains anti-oxidant Si-Zr-Y infiltration layer on material sample.
The surface that described wish is made the material sample of infiltration layer adopts 80～1000#SiC liquid honing ultrasonic cleaning drying up in dehydrated alcohol.
While having the material sample of multiple infiltration layers in crucible in described step 3, the distance between adjacent parallel material sample is not less than 15mm.
Described Si≤200 order.
Described Zr≤200 order.
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, efficiency advantages of higher.Adopt 1250 DEG C of constant temperature oxidation experiments to detect, ooze altogether rear sample through the densification of 100h constant temperature oxidation rear oxidation film, rare coming off, shows 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, efficiency advantages of higher, be suitable for produce and application.
Brief description of the drawings
Fig. 1: technical process of the present invention;
Fig. 2: ooze altogether the macro morphology figure on co-penetration layer surface under condition for the difference that adopts the present invention to obtain, wherein the temperature of oozing altogether of Fig. 2 (a) is 1000 DEG C, and the time of oozing is 1h altogether, and 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 DEG C, and the time of oozing is 5h altogether, and 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 DEG C, and the time of oozing is 12h altogether, and 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 condition for the difference that adopts the present invention to obtain, wherein the temperature of oozing altogether of Fig. 3 (a) is 1000 DEG C, and the time of oozing is 1h altogether, and 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 DEG C, and the time of oozing is 5h altogether, and 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 DEG C, and the time of oozing is 12h altogether, and 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 condition for the difference that adopts the present invention to obtain, wherein the temperature of oozing altogether of Fig. 4 (a) is 1000 DEG C, and the time of oozing is 1h altogether, and 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 DEG C, and the time of oozing is 5h altogether, and 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 DEG C, and the time of oozing is 12h altogether, and 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 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 DEG C, and the time of oozing is 1h altogether, and 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 DEG C, and the time of oozing is 5h altogether, and 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 DEG C, and the time of oozing is 12h altogether, and penetration enhancer component is 25Si-15Zr-5Y
2o
3-8NaF-47Al
2o
3(wt%);
Fig. 6: be the macro morphology of the sample after 1250 DEG C/5h oozes altogether after 1250 DEG C of constant temperature oxidation 100h.
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 alcohol through the each face of 1000# sand papering, dries up for subsequent use; 2. prepare penetration enhancer: accurately take according to quantity penetration enhancer, the proportioning of penetration enhancer is by weight percentage: 200 object silicon, content is 10%, 200 object zirconiums, content is 5%, 200 object yttrium oxide, content is 1%, Sodium Fluoride is analytical pure (99%), content 3%, and all the other are for being 200 object aluminium sesquioxides; 3. ball milling: the penetration enhancer preparing is placed in to satellite gear ball mill spheroidal graphite 4h, its abundant refinement is mixed; 4. fill sample: pack the penetration enhancer after ball milling into crucible, and sample is imbedded in penetration enhancer and compacting, the distance between adjacent parallel sample is not less than 15mm, and the penetration enhancer thickness that specimen surface covers is not less than 10mm; 5. sealing: silicon sol and Al are added a cover and used to the crucible that sample is housed
2o
3, Y
2o
3and ZrO
2powder-tight is placed on the diffusion of high temperature high vacuum controlled atmosphere and oozes in stove; 6. diffusion is oozed: system is evacuated down to 3.0 × 10
-2after Pa, start to heat with the temperature rise rate of 18 DEG C/min, applying argon gas protection while being heated to 450 DEG C, temperature is incubated 1h while rising to 1000 DEG C, then close heating system, and sample is chilled to room temperature with stove; 7. cleaning, drying: the sample after oozing is altogether used to alcohol ultrasonic irrigation 15min, then dry, finish.
Embodiment 2
1. prepare sample: sample is placed on ultrasonic cleaning in alcohol through the each face of 1000# sand papering, dries up for subsequent use; 2. prepare penetration enhancer: accurately take according to quantity penetration enhancer, the proportioning of penetration enhancer is by weight percentage: 200 object silicon, content is 15%, 200 object zirconiums, content is 10%, 200 object yttrium oxide, content is 3%, Sodium Fluoride is analytical pure (99%), content 5%, and all the other are for being 200 object aluminium sesquioxides; 3. ball milling: the penetration enhancer preparing is placed in to satellite gear ball mill spheroidal graphite 4h, its abundant refinement is mixed; 4. fill sample: pack the penetration enhancer after ball milling into crucible, and sample is imbedded in penetration enhancer and compacting, the distance between adjacent parallel sample is not less than 15mm, and the penetration enhancer thickness that specimen surface covers is not less than 10mm; 5. sealing: silicon sol and Al are added a cover and used to the crucible that sample is housed
2o
3, Y
2o
3and ZrO
2powder-tight is placed on the diffusion of high temperature high vacuum controlled atmosphere and oozes in stove; 6. diffusion is oozed: system is evacuated down to 3.0 × 10
-2after Pa, start to heat with the temperature rise rate of 18 DEG C/min, applying argon gas protection while being heated to 450 DEG C, temperature is incubated 5h while rising to 1250 DEG C, then close heating system, and sample is chilled to room temperature with stove; 7. cleaning, drying: the sample after oozing is altogether used to alcohol ultrasonic irrigation 15min, then dry, finish.
Embodiment 3:
1. prepare sample: sample is placed on ultrasonic cleaning in alcohol through the each face of 1000# sand papering, dries up for subsequent use; 2. prepare penetration enhancer: accurately take according to quantity penetration enhancer, the proportioning of penetration enhancer is by weight percentage: 200 object silicon, content is 25%, 200 object zirconiums, content is 15%, 200 object yttrium oxide, content is 5%, Sodium Fluoride is analytical pure (99%), content 8%, and all the other are for being 200 object aluminium sesquioxides; 3. ball milling: the penetration enhancer preparing is placed in to satellite gear ball mill spheroidal graphite 4h, its abundant refinement is mixed; 4. fill sample: pack the penetration enhancer after ball milling into crucible, and sample is imbedded in penetration enhancer and compacting, the distance between adjacent parallel sample is not less than 15mm, and the penetration enhancer thickness that specimen surface covers is not less than 10mm; 5. sealing: silicon sol and Al are added a cover and used to the crucible that sample is housed
2o
3, Y
2o
3and ZrO
2powder-tight is placed on the diffusion of high temperature high vacuum controlled atmosphere and oozes in stove; 6. diffusion is oozed: system is evacuated down to 3.0 × 10
-2after Pa, start to heat with the temperature rise rate of 18 DEG C/min, applying argon gas protection while being heated to 450 DEG C, temperature is incubated 12h while rising to 1400 DEG C, then close heating system, and sample is chilled to room temperature with stove; 7. cleaning, drying: the sample after oozing is altogether used to alcohol ultrasonic irrigation 15min, then dry, finish.
Claims (7)
1. a preparation method for the anti-oxidant Si-Zr-Y infiltration layer of Nb-Ti-Si base alloy surface, 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, and skin, transition layer and the every one deck of internal layer all contain Zr; 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
3preparation penetration enhancer;
Step 2: the penetration enhancer preparing is placed in to ball mill and carries out 4h ball milling, drum's speed of rotation is 360 turn/min;
Step 3: pack the penetration enhancer after ball milling into crucible, then the material sample that wish is made infiltration layer is imbedded in penetration enhancer and compacting, the penetration enhancer thickness that specimen surface covers is not less than 10mm; While having the material sample of multiple infiltration layers in crucible in described step 3, the distance between adjacent parallel material sample is not less than 15mm;
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 stove; Described sealing material is silicon sol and Al
2o
3, Y
2o
3and ZrO
2the mixture of powder, ratio is 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
-2after Pa, start to heat with the temperature rise rate of 18 DEG C/min, applying argon gas protection while being heated to 450 DEG C, temperature is incubated 1-12h while rising to 1000-1400 DEG C, then close heating system and be chilled to room temperature with stove;
Step 6: the material sample after diffusion is oozed, ultrasonic cleaning 15 minutes, is then dried, and obtains anti-oxidant Si-Zr-Y infiltration layer on material sample.
2. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of Nb-Ti-Si base alloy surface according to claim 1, is characterized in that: the surface that described wish is made the material sample of infiltration layer adopts 80～1000#SiC liquid honing ultrasonic cleaning drying up in dehydrated alcohol.
3. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of Nb-Ti-Si base alloy surface according to claim 1, is characterized in that: described Si≤200 order.
4. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of Nb-Ti-Si base alloy surface according to claim 1, is characterized in that: described Zr≤200 order.
5. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of Nb-Ti-Si base alloy surface according to claim 1, is characterized in that: described Y
2o
3≤ 200 orders.
6. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of Nb-Ti-Si base alloy surface according to claim 1, is characterized in that: described Al
2o
3≤ 200 orders.
7. the preparation method of the anti-oxidant Si-Zr-Y infiltration layer of Nb-Ti-Si base alloy surface according to claim 1, is characterized in that: it is analytical pure that described NaF adopts rank.
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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 |
| CN103949590B (en) * | 2014-05-12 | 2016-06-29 | 西北工业大学 | A kind of oxide doped and modified Y2O3The preparation method of+YSZ is high temperature resistant shell |
| 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 |
| CN106435460B (en) * | 2016-10-18 | 2018-10-12 | 中国矿业大学 | A kind of niobium alloy surface high-temp wear-resistant 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 |
| 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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