CN104788106B - The manufacture method of vacuum induction melting high temperature alloy crucible - Google Patents
The manufacture method of vacuum induction melting high temperature alloy crucible Download PDFInfo
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Abstract
The present invention provides a kind of manufacture method of vacuum induction melting high temperature alloy crucible, and step is：1) raw material by fused alumina zirconia, the fused alumina zirconia of 0.1 1mm, the fused alumina zirconia of below 0.1mm, bimodal activity alpha-aluminium oxide and nanocrystalline alpha-aluminium oxide that particle size is 1 4mm with 15 40：15‑40：15‑40：3‑8：38 mass percent is mixed, then raw material and ammonium polyacrylate and bonding agent are mixed to obtain into slurry, and wherein ammonium polyacrylate, bonding agent addition is respectively the 0.5 2% and 5 15% of raw material gross mass；2) by slurry gross mass is added in slurry 0.1 0.3% water solubility 2,2' azos hydrochloride or piperidine hydrochlorate, 3 10min are mixed at 2 30 DEG C；3) by step 2) obtain slurry crucible mould is poured into after 2 30 DEG C of vacuum outgas 5min, immediately；4) together with mould be heated to 45 55 DEG C keep 5 35min after the demoulding, by crucible base substrate drying at room temperature；5) crucible base substrate is placed in more than 1,500 1650 DEG C of retention time 3h, is subsequently cooled to room temperature and obtains final product object.Using crucible obtained in the present invention, in melting high temperature alloy, impurity content is low.
Description
Technical field
The present invention relates to a kind of manufacture method of vacuum induction melting high temperature alloy crucible, belong to metallurgical technology field.
Background technology
Critical component when crucible is vacuum induction melting high temperature alloy.Under high temperature and vacuum condition, crucible and high temperature
Various physics chemical actions can occur between alloy melt, as a result will cause that crucible material is etched, melt is contaminated.Therefore,
It is required that crucible material should have good chemical stability.Meanwhile, crucible periodically undergoes plus hot and cold in use
But effect, produces expansion and shrinkage stress inside crucible, so as to crack, causes melt leakage, it is therefore desirable to crucible
Material has good thermal shock resistance.
The impurity elements such as oxygen, nitrogen, sulphur, phosphorus are interfered significantly on to the mechanical property of high temperature alloy.Nitrogen is in high temperature alloy
Exist generally in the form of nitride or carbonitride, these compounds are highly stable, will not be under common smelting temperature
Melted in melt, to reduce the nitrogen content in high temperature alloy, it is necessary to use smelting temperature higher, so further exacerbate
Physics chemical action between crucible and melt, causes to a greater degree of pollution of melt.
At present, the crucible material that vacuum induction melting high temperature alloy is used mainly magnesia crucible, but due to oxidation
Magnesium carbon, aluminium, titanium, niobium, chromium isoreactivity element in meeting under high temperature and high vacuum are acted on is by high temperature alloy are reduced and pollute alloy,
It is difficult to further reduce the degree of purity of high temperature alloy.To overcome the shortcoming of magnesia crucible, test steady using high temeperature chemistry
The qualitative calcareous crucible for smelting high temperature alloy of oxidation higher, but due to calcium oxide, to there is easy aquation, not easy-formation and cost high etc.
Shortcoming, industrial applications are not obtained.Pure corundum (aluminum oxide) matter crucible chemical stability is good, at high temperature with high temperature alloy
Melt will not chemically react, and can be used to the high-purity high temperature alloy of melting.But due to existing pure corundum crucible, its thermal shock
Stability is poor, easy to crack, can't be used as vacuum induction melting high temperature alloy crucible.To overcome the shortcomings of pure corundum crucible,
Chinese patent (ZL 201210440801.0) discloses a kind of corundum spinel crucible and preparation method thereof, because magnalium point is brilliant
The high volume stability and thermal shock resistance of stone are better than magnesia material, and thermal shock resistance is better than corundum, corrosion resistance and antioxygen
Change reproducibility and be better than mullite, there is excellent applied at elevated temperature performance with its crucible for preparing, but still containing purer in its composition
The composition of corundum stability at elevated temperature difference is present.
The content of the invention
Closed it is an object of the invention to provide a kind of vacuum induction melting high temperature that can overcome drawbacks described above, excellent working performance
The manufacture method of gold crucible, its technical scheme is：
A kind of manufacture method of vacuum induction melting high temperature alloy crucible, it is characterised in that comprise the following steps：
1) raw material components are by mass percentage：Particle size is the fused alumina zirconia 15-40% of 1-4mm, particle size is
The fused alumina zirconia 15-40% of 0.1-1mm, particle size are fused alumina zirconia 15-40%, the bimodal activity Alpha-alumina 3- of below 0.1mm
8% and nanocrystalline Alpha-alumina 3-8%；Dispersant is ammonium polyacrylate；Bonding agent is acrylamide and N, N '-di-2-ethylhexylphosphine oxide third
The mixed aqueous solution of acrylamide, the mass ratio of the two is 10:1, the total mass percent concentration of mixed aqueous solution is 14%；By original
Material, dispersant, bonding agent are with 100：0.5-2：The mass ratio of 5-15 is well mixed to obtain slurry；
2) by step 1) initiator is added in the slurry that obtains, 3-10min is mixed at 2-30 DEG C, initiator is water-soluble 2,
2'- azos hydrochloride or piperidine hydrochlorate, addition are the 0.1-0.3% of slurry gross mass；
3) by step 2) obtain slurry crucible mould is poured into after 2-30 DEG C of vacuum outgas 5min, immediately, wherein
Devolatilization vacuum degree is less than 10Pa；
4) together with mould be heated to 45-55 DEG C keep 5-35min after the demoulding, by crucible base substrate drying at room temperature；
5) by dried crucible base substrate be placed in kiln sinter, sintering temperature be 1500-1650 DEG C, retention time 3h with
On, it is subsequently cooled to room temperature and obtains vacuum induction melting high temperature alloy crucible.
Compared with prior art, its advantage is the present invention：Vacuum induction melting high temperature alloy crucible disclosed by the invention
It is raw material from fused alumina zirconia, using special technique moulding by casting, the α-Al2O3 for constituting mutually for corundum structure of finished product crucible,
The Tetragonal t-ZrO2 of the square structure and monoclinic phase m-ZrO2 of monocline, stability at elevated temperature and thermal shock resistance are good；
The shaping adjuvant used not sulfur-bearing of crucible and phosphorus, sulphur and phosphorus will not be increased during melting high temperature alloy to melt；Addition bimodal activity α-oxygen
Change aluminium and nanocrystalline Alpha-alumina, and burnt till through 1500-1650 DEG C of high temperature, bond strength is high, and anti-melt scouring capability is strong.Using
Crucible for smelting high temperature alloy of the present invention, can carry out the impurity such as more than 1700 DEG C melt high-temperature process, alloy O, N, S, P of melting
Constituent content is low.
Specific embodiment
With reference to embodiment, the present invention is further described.
The quality proportioning of raw material is shown in Table 1 in each embodiment.
Embodiment 1
The manufacture of vacuum induction melting high temperature alloy crucible is comprised the following steps：
1) uniform slurry is mixed to get with dispersant and bonding agent after being weighed by the proportioning of table 1, dispersant used is poly-
Ammonium acrylate, addition is the 0.5% of raw material gross mass, and bonding agent is acrylamide and N, N '-methylene-bisacrylamide
Mixed aqueous solution, the quality proportioning of the two is 10:1, the total mass percent concentration of mixed aqueous solution be 14%, bonding agent plus
It is the 5% of raw material gross mass to enter amount；
2) by step 1) obtain slurry in add initiator, 30 DEG C mix 3min, initiator be water solubility 2,2'- idols
Nitrogen salt hydrochlorate, addition is the 0.3% of slurry gross mass；
3) by step 2) obtain slurry in 30 DEG C of vacuum outgas 5min, crucible mould is poured into immediately, wherein deaerating
Vacuum 9Pa；
4) together with mould be heated to 45 DEG C keep 30min after the demoulding, then in drying at room temperature；
5) dried crucible base substrate is placed in kiln and is sintered, sintering temperature is 1650 DEG C, retention time 3.5h, then
It is cooled to room temperature and obtains vacuum induction melting high temperature alloy crucible.
Embodiment 2
The manufacture of vacuum induction melting high temperature alloy crucible is comprised the following steps：
1) uniform slurry is mixed to get with dispersant and bonding agent after being weighed by the proportioning of table 1, dispersant used is poly-
Ammonium acrylate, addition is the 1.5% of raw material gross mass, and bonding agent is acrylamide and N, N '-methylene-bisacrylamide
Mixed aqueous solution, the quality proportioning of the two is 10:1, the total mass percent concentration of mixed aqueous solution be 14%, bonding agent plus
It is the 10% of raw material gross mass to enter amount；
2) by step 1) obtain slurry in add initiator, 25 DEG C mix 6min, initiator is piperidine hydrochlorate, plus
It is the 0.2% of slurry gross mass to enter amount；
3) by step 2) obtain slurry in 25 DEG C of vacuum outgas 5min, crucible mould is poured into immediately, wherein deaerating
Vacuum 8Pa；
4) 50 DEG C of holding 35min demouldings are heated to together with mould, then in drying at room temperature；
5) dried crucible base substrate is placed in kiln and is sintered, sintering temperature is 1600 DEG C, retention time 4h, Ran Houleng
But vacuum induction melting high temperature alloy crucible is obtained to room temperature.
Embodiment 3
The manufacture of vacuum induction melting high temperature alloy crucible is comprised the following steps：
1) uniform slurry is mixed to get with dispersant and bonding agent after being weighed by the proportioning of table 1, dispersant used is poly-
Ammonium acrylate, addition is the 2% of raw material gross mass, and bonding agent is the mixed of acrylamide and N, N '-methylene-bisacrylamide
Heshui solution, the quality proportioning of the two is 10:1, the total mass percent concentration of mixed aqueous solution is 14%, the addition of bonding agent
Measure is the 15% of raw material gross mass；
2) by step 1) obtain slurry in add initiator, 20 DEG C mix 8min, initiator is 2,2'- azo hydrochloric acid
Salt, addition is the 0.15% of slurry gross mass；
3) by step 2) obtain slurry in 20 DEG C of vacuum outgas 5min, crucible mould is poured into immediately, wherein deaerating
Vacuum 7Pa；
4) 55 DEG C of holding 35min demouldings are heated to together with mould, then in drying at room temperature；
5) dried crucible base substrate is placed in kiln and is sintered, sintering temperature is 1500 DEG C, retention time 5h, Ran Houleng
But vacuum induction melting high temperature alloy crucible is obtained to room temperature.
Embodiment 4
1) uniform slurry is mixed to get with dispersant and bonding agent after being weighed by the proportioning of table 1, dispersant used is poly-
Ammonium acrylate, addition is the 1% of raw material gross mass, and bonding agent is the mixed of acrylamide and N, N '-methylene-bisacrylamide
Heshui solution, the quality proportioning of the two is 10:1, the total mass percent concentration of mixed aqueous solution is 14%, the addition of bonding agent
Measure is the 8% of raw material gross mass；
2) by step 1) obtain slurry in add initiator, 15 DEG C mix 10min, initiator is piperidine hydrochlorate,
Addition is the 0.1% of slurry gross mass；
3) by step 2) obtain slurry in 15 DEG C of vacuum outgas 5min, crucible mould is poured into immediately, wherein deaerating
Vacuum 6Pa；
4) 55 DEG C of holding 35min demouldings are heated to together with mould, then in drying at room temperature；
5) dried crucible base substrate is placed in kiln and is sintered, sintering temperature is 1550 DEG C, retention time 5h, Ran Houleng
But vacuum induction melting high temperature alloy crucible is obtained to room temperature.
Embodiment 5
The manufacture of vacuum induction melting high temperature alloy crucible is comprised the following steps：
1) uniform slurry is mixed to get with dispersant and bonding agent after being weighed by the proportioning of table 1, dispersant used is poly-
Ammonium acrylate, addition is the 1.5% of raw material gross mass, and bonding agent is acrylamide and N, N '-methylene-bisacrylamide
Mixed aqueous solution, the quality proportioning of the two is 10:1, the total mass percent concentration of mixed aqueous solution be 14%, bonding agent plus
It is the 12% of raw material gross mass to enter amount；
2) by step 1) obtain slurry in add initiator, 15 DEG C mix 10min, initiator is 2,2'- diazo salts
Hydrochlorate, addition is the 0.2% of slurry gross mass；
3) by step 2) obtain slurry in 15 DEG C of vacuum outgas 5min, crucible mould is poured into immediately, wherein deaerating
Vacuum 6Pa；
4) 50 DEG C of holding 20min demouldings are heated to together with mould, then in drying at room temperature；
5) dried crucible base substrate is placed in kiln and is sintered, sintering temperature is 1580 DEG C, retention time 5h, Ran Houleng
But vacuum induction melting high temperature alloy crucible is obtained to room temperature.
Embodiment 6
The manufacture of vacuum induction melting high temperature alloy crucible is comprised the following steps：
1) uniform slurry is mixed to get with dispersant and bonding agent after being weighed by the proportioning of table 1, dispersant used is poly-
Ammonium acrylate, addition is the 2% of raw material gross mass, and bonding agent is the mixed of acrylamide and N, N '-methylene-bisacrylamide
Heshui solution, the quality proportioning of the two is 10:1, the total mass percent concentration of mixed aqueous solution is 14%, the addition of bonding agent
Measure is the 10% of raw material gross mass；
2) by step 1) obtain slurry in add initiator, 25 DEG C mix 5min, initiator is piperidine hydrochlorate, plus
It is the 0.25% of slurry gross mass to enter amount；
3) by step 2) obtain slurry in 25 DEG C of vacuum outgas 5min, crucible mould is poured into immediately, wherein deaerating
Vacuum 9Pa；
4) 45 DEG C of holding 30min demouldings are heated to together with mould, then in drying at room temperature；
5) dried crucible base substrate is placed in kiln and is sintered, sintering temperature is 1650 DEG C, retention time 5h, Ran Houleng
But vacuum induction melting high temperature alloy crucible is obtained to room temperature.
Embodiment 7
The manufacture of vacuum induction melting high temperature alloy crucible is comprised the following steps：
1) uniform slurry is mixed to get with dispersant and bonding agent after being weighed by the proportioning of table 1, dispersant used is poly-
Ammonium acrylate, addition is the 2% of raw material gross mass, and bonding agent is the mixed of acrylamide and N, N '-methylene-bisacrylamide
Heshui solution, the quality proportioning of the two is 10:1, the total mass percent concentration of mixed aqueous solution is 14%, the addition of bonding agent
Measure is the 8% of raw material gross mass；
2) by step 1) obtain slurry in add initiator, 30 DEG C mix 8min, initiator is 2,2'- azo hydrochloric acid
Salt, addition is the 0.2% of slurry gross mass；
3) by step 2) obtain slurry in 30 DEG C of vacuum outgas 5min, crucible mould is poured into immediately, wherein deaerating
Vacuum 9Pa；
4) together with mould be heated to 50 DEG C keep 15min after the demoulding, then in drying at room temperature；
5) dried crucible base substrate is placed in kiln and is sintered, sintering temperature is 1600 DEG C, retention time 3.5h, then
It is cooled to room temperature and obtains vacuum induction melting high temperature alloy crucible.
Embodiment 8
The manufacture of vacuum induction melting high temperature alloy crucible is comprised the following steps：
1) uniform slurry is mixed to get with dispersant and bonding agent after being weighed by the proportioning of table 1, dispersant used is poly-
Ammonium acrylate, addition is the 1.5% of raw material gross mass, and bonding agent is acrylamide and N, N '-methylene-bisacrylamide
Mixed aqueous solution, the quality proportioning of the two is 10:1, the total mass percent concentration of mixed aqueous solution be 14%, bonding agent plus
It is the 10% of raw material gross mass to enter amount；
2) by step 1) obtain slurry in add initiator, 2 DEG C mix 3min, initiator is piperidine hydrochlorate, plus
It is the 0.2% of slurry gross mass to enter amount；
3) by step 2) slurry that obtains, in 2 DEG C of vacuum outgas 5min, pours into crucible mould, wherein degassing is true immediately
Reciprocal of duty cycle 5Pa；
4) together with mould be heated to 50 DEG C keep 20min after the demoulding, then in drying at room temperature；
5) dried crucible base substrate is placed in kiln and is sintered, sintering temperature is 1620 DEG C, retention time 4h, Ran Houleng
But vacuum induction melting high temperature alloy crucible is obtained to room temperature.
Embodiment 9
The manufacture of vacuum induction melting high temperature alloy crucible is comprised the following steps：
1) uniform slurry is mixed to get with dispersant and bonding agent after being weighed by the proportioning of table 1, dispersant used is poly-
Ammonium acrylate, addition is the 2% of raw material gross mass, and bonding agent is the mixed of acrylamide and N, N '-methylene-bisacrylamide
Heshui solution, the quality proportioning of the two is 10:1, the total mass percent concentration of mixed aqueous solution is 14%, the addition of bonding agent
Measure is the 10% of raw material gross mass；
2) by step 1) obtain slurry in add initiator, 10 DEG C mix 5min, initiator is 2,2'- azo hydrochloric acid
Salt, addition is the 0.2% of slurry gross mass；
3) by step 2) obtain slurry in 10 DEG C of vacuum outgas 5min, crucible mould is poured into immediately, wherein deaerating
Vacuum 9Pa；
4) together with mould be heated to 50 DEG C keep 15min after the demoulding, then in drying at room temperature；
5) dried crucible base substrate is placed in kiln and is sintered, sintering temperature is 1500 DEG C, retention time 5h, Ran Houleng
But vacuum induction melting high temperature alloy crucible is obtained to room temperature.
Embodiment 10
The manufacture of vacuum induction melting high temperature alloy crucible is comprised the following steps：
1) uniform slurry is mixed to get with dispersant and bonding agent after being weighed by the proportioning of table 1, dispersant used is poly-
Ammonium acrylate, addition is the 1.5% of raw material gross mass, and bonding agent is acrylamide and N, N '-methylene-bisacrylamide
Mixed aqueous solution, the quality proportioning of the two is 10:1, the total mass percent concentration of mixed aqueous solution be 14%, bonding agent plus
It is the 12% of raw material gross mass to enter amount；
2) by step 1) obtain slurry in add initiator, 15 DEG C mix 7min, initiator is piperidine hydrochlorate, plus
It is the 0.2% of slurry gross mass to enter amount；
3) by step 2) obtain slurry in 15 DEG C of vacuum outgas 5min, crucible mould is poured into immediately, wherein deaerating
Vacuum 8Pa；
4) together with mould be heated to 50 DEG C keep 5min after the demoulding, then in drying at room temperature；
5) dried crucible base substrate is placed in kiln and is sintered, sintering temperature is 1650 DEG C, retention time 4h, Ran Houleng
But vacuum induction melting high temperature alloy crucible is obtained to room temperature.
The crucible made using embodiment is carried out vacuum induction melting, vacuum pouring nickel-base cast superalloy K417 and tried
Test, 1750 DEG C of melt high-temperature process are used in fusion process.Sampled from the alloy pig of cast, using TC-436 oxygen-nitrogen analyzers
Analysis oxygen and nitrogen content, the results are shown in Table 2.It can be seen that, using the gas content in the nickel-base cast superalloy of crucible for smelting of the present invention
It is very low.
The proportioning (mass percent) of raw material in each embodiment of table 1
Table 2 using crucible vacuum induction melting of the present invention nickel-base cast superalloy K417 in oxygen and nitrogen content (×
0.0001%, mass percent)
| Embodiment | Oxygen | Nitrogen |
| Embodiment 1 | 4 | 3 |
| Embodiment 2 | 6 | 5 |
| Embodiment 3 | 5 | 4 |
| Embodiment 4 | 6 | 5 |
| Embodiment 5 | 5 | 4 |
| Embodiment 6 | 4 | 3 |
| Embodiment 7 | 6 | 5 |
| Embodiment 8 | 5 | 4 |
| Embodiment 9 | 6 | 5 |
| Embodiment 10 | 6 | 3 |
Claims (1)
1. a kind of manufacture method of vacuum induction melting high temperature alloy crucible, it is characterised in that comprise the following steps：
1) raw material components are by mass percentage：Particle size is the fused alumina zirconia 15-40% of 1-4mm, particle size is 0.1-
The fused alumina zirconia 15-40% of 1mm, particle size for below 0.1mm fused alumina zirconia 15-40%, bimodal activity Alpha-alumina 3-8% and
Nanocrystalline Alpha-alumina 3-8%；Dispersant is ammonium polyacrylate；Bonding agent is acrylamide and N, N '-methylene bisacrylamide acyl
The mixed aqueous solution of amine, the mass ratio of the two is 10:1, the total mass percent concentration of mixed aqueous solution is 14%；By raw material,
Dispersant, bonding agent are with 100：0.5-2：The mass ratio of 5-15 is well mixed to obtain slurry；
2) by step 1) initiator is added in the slurry that obtains, 3-10min is mixed at 2-30 DEG C, initiator is water-soluble 2,2'-
Azo hydrochloride or piperidine hydrochlorate, addition are the 0.1-0.3% of slurry gross mass；
3) by step 2) obtain slurry crucible mould is poured into after 2-30 DEG C of vacuum outgas 5min, immediately, wherein deaerating
Vacuum is less than 10Pa；
4) together with mould be heated to 45-55 DEG C keep 5-35min after the demoulding, by crucible base substrate drying at room temperature；
5) dried crucible base substrate is placed in kiln and is sintered, sintering temperature is 1500-1650 DEG C, more than retention time 3h,
It is subsequently cooled to room temperature and obtains vacuum induction melting high temperature alloy crucible.
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| CN112809010A (en) * | 2020-12-29 | 2021-05-18 | 辽宁冠达新材料科技有限公司 | Preparation method of GH5188 cobalt-based high-temperature alloy powder for 3D printing |
| CN113480295A (en) * | 2021-08-04 | 2021-10-08 | 中钢集团洛阳耐火材料研究院有限公司 | Ceramic crucible for nickel-based high-temperature alloy and preparation method |
| CN116177999A (en) * | 2022-12-16 | 2023-05-30 | 中航装甲科技有限公司 | Alumina crucible for high-temperature alloy smelting and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4778778A (en) * | 1987-06-03 | 1988-10-18 | Keramont Advanced Ceramic Products Corporation | Process for the production of sintered aluminum nitrides |
| CN101928143A (en) * | 2010-08-24 | 2010-12-29 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of high-purity zirconia refractory product |
| CN102951913A (en) * | 2012-11-08 | 2013-03-06 | 中山市华山特种陶瓷有限公司 | Isostatic compaction corundum spinel crucible and preparation method thereof |
| CN103848624A (en) * | 2012-11-29 | 2014-06-11 | 洛阳中苑陶瓷科技有限公司 | Preparation method of fused alumina zirconia ceramic crucible |
-
2015
- 2015-03-18 CN CN201510117836.4A patent/CN104788106B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4778778A (en) * | 1987-06-03 | 1988-10-18 | Keramont Advanced Ceramic Products Corporation | Process for the production of sintered aluminum nitrides |
| CN101928143A (en) * | 2010-08-24 | 2010-12-29 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of high-purity zirconia refractory product |
| CN102951913A (en) * | 2012-11-08 | 2013-03-06 | 中山市华山特种陶瓷有限公司 | Isostatic compaction corundum spinel crucible and preparation method thereof |
| CN103848624A (en) * | 2012-11-29 | 2014-06-11 | 洛阳中苑陶瓷科技有限公司 | Preparation method of fused alumina zirconia ceramic crucible |
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