CN102071333B - Method for preparing foamed TiAl intermetallic compound - Google Patents
Method for preparing foamed TiAl intermetallic compound Download PDFInfo
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- CN102071333B CN102071333B CN2010105957321A CN201010595732A CN102071333B CN 102071333 B CN102071333 B CN 102071333B CN 2010105957321 A CN2010105957321 A CN 2010105957321A CN 201010595732 A CN201010595732 A CN 201010595732A CN 102071333 B CN102071333 B CN 102071333B
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Abstract
The invention discloses a method for preparing a foamed TiAl intermetallic compound. The method comprises the following steps of: adding 15 to 35 percent of low-temperature decomposition temperature pore-forming agent, 10 to 40 percent of moderate-temperature decomposition temperature pore-forming agent and 5 to 35 percent of high-temperature decomposition temperature pore-forming agent accordingto the total volume of 100 percent of mixed powder of TiAl powder and the pore-forming agents; uniformly mixing and performing compression molding; heating under vacuum; preserving heat at a low-temperature stage, a moderate-temperature stage and a high-temperature stage respectively; removing the pore-forming agents in turn; and sintering to obtain a high-porosity foamed TiAl intermetallic compound material with certain strength. The prepared TiAl intermetallic compound porous material has the porosity of over 80 percent, certain structural strength, high porosity, a simple and controllable process, stable quality and high repeatability, contributes to large-scale production and is suitable for the field of high-temperature heat insulation.
Description
Technical field
The invention discloses a kind of preparation method of foam TiAl intermetallic compound, be specifically related to add the method that composite pore-forming agent prepares foam TiAl inter-metallic compound material.The foam metal material preparing technical field.
Background technology
The TiAl intermetallic compound is a kind of type material between pottery and metallic substance, has excellent material property, like low density; High Young's modulus, high thermal conductivity, high specific tenacity and specific rigidity; Excellent high temperature oxidation resistance; Good anti-various strong acid, highly basic, salt fog, chlorine molecule and chloride ion corrosion performance, and workability etc., considerable application prospect had.
At present, the pore-forming material that is used for preparing porous material mainly contains polymethylmethacrylate (PMMA), polyvinyl butyral acetal (PVB) and methylcellulose gum etc., is confined to middle low temperature (below 500 ℃) one-step removal mostly.This method mainly is used for preparing porous ceramic film material and a part of porous metal, and the porosity of prepared porous material is mostly in 30%～50% scope.
The TiAl intermetallic compound porous material is to adopt the reaction synthesis method preparation at present.Reaction synthesis method be a kind of be raw material with the element powders, in powder sintered process, utilize the partially Kirkendall effect that causes of diffusion of Al element, in material, produce a certain amount of Frenkel hole, prepare the TiAl intermetallic compound porous material.The porosity of the TiAl intermetallic compound porous material of preparation is 20%～50% thus, is applied to fields such as filtration, separation and purification.
The TiAl intermetallic compound is a kind of high-temperature material, at 800 ℃ good thermotolerance is arranged.But, the TiAl intermetallic compound porous material of reaction synthesis method preparation, porosity is lower, and thermal conductivity is higher, makes it be difficult to be applied to fields such as heat insulation and sound insulation.Because fields such as heat insulation and sound insulation require highly porous material.
Summary of the invention
The present invention aims to provide a kind of preparation method of foam TiAl intermetallic compound; Through design composite pore-forming agent series; Comprise pore-forming material serial selection, content, remove mode and technology, finally prepare porosity up to the foam TiAl intermetallic compound more than 80%.
The preparation method of a kind of foam TiAl of the present invention intermetallic compound comprises the steps:
The first step: getting granularity is 100～400 purpose Ti powder, Al powder, is the Ti powder by mass percentage: Al powder=(40～80): mix (20～60); Then, be 100% by the mixed powder TV of Ti Al powder and pore-forming material, add the low-temperature decomposition temperature pore-forming material that accounts for mixed powder TV 15%～35%; Add the middle temperature decomposition temperature pore-forming material that accounts for mixed powder TV 10%～40%; Add the high-temperature decomposition temperature pore-forming material that accounts for mixed powder TV 5%～35%; Ball mill mixing is even; Obtain the mixture of Ti powder, Al powder and pore-forming material;
Second step: with the first step gained mixture compression moulding post-heating, vacuum tightness is 1.0 * 10 in the control stove
-1～1.0 * 10
-3Pa is incubated respectively by low thermophase, middle thermophase, hot stage, removes low-temperature decomposition temperature pore-forming material, middle temperature decomposition temperature pore-forming material, high-temperature decomposition temperature pore-forming material successively; Obtain the Ti Al powder mold pressing base of high porosity; Then, be heated to sintering temperature and carry out sintering, the porosity that promptly obtains having certain intensity is up to the foam TiAl inter-metallic compound material more than 80%; The heating cycle of sintering process is: 10～20 ℃/min of rate of heating, 1200～1400 ℃ of sintering temperatures, soaking time 120～180min.
Among the preparation method of a kind of foam TiAl of the present invention intermetallic compound, said low-temperature decomposition temperature pore-forming material is selected from least a in bicarbonate of ammonia, the volatile salt; Warm decomposition temperature pore-forming material is selected from least a in urea, the Zinic stearas in said; Said high-temperature decomposition temperature pore-forming material is selected from least a in lime carbonate, the magnesiumcarbonate.
Among the preparation method of a kind of foam TiAl of the present invention intermetallic compound, said low thermophase heating cycle is: 5～10 ℃/min of rate of heating, 50～100 ℃ of holding temperatures, soaking time 30～120min; The thermophase heating cycle is in said: 2～10 ℃/min of rate of heating, 150～350 ℃ of holding temperatures, soaking time 60～120min; Said hot stage heating cycle is: 2～5 ℃/min of rate of heating, 500～1000 ℃ of holding temperatures, soaking time 60～120min.
Among the preparation method of a kind of foam TiAl of the present invention intermetallic compound, the ball-to-powder weight ratio of said ball mill mixing is (2～10): 1, and mixing time 4h～12h.
Among the preparation method of a kind of foam TiAl of the present invention intermetallic compound, a kind of in isostatic cool pressing, the mold pressing adopted in said compression moulding, and pressing pressure is 50MPa～400MPa.
The present invention is a raw material with Ti, Al element powders; Design and interpolation have different decomposition temperature, different volumes fractional composite pore-forming agent; Mode mixing through ball mill mixing; And be shaped through the mode of colding pressing, under vacuum atmosphere, carry out interim degreasing subsequently after, finally prepare highly porous foam TiAl intermetallic compound through high-sintering process.The purpose of adding composite pore-forming agent mainly is; Can remove pore-forming material stage by stage,, guarantee that pore-forming material progressively removes fully promptly through design skimming temp and time; Can guarantee the stable of porous insert pore structure like this and do not subside; Then through follow-up high temperature sintering, prepare the porosity with certain intensity and compare with existing reaction synthesis method up to the foam TiAl inter-metallic compound material more than 80%, present method has following advantage:
(1) porosity of prepared TiAl intermetallic compound porous material has been broken through original 20%～50% restriction, can prepare porosity up to compound-material between the foamed metal more than 80%, can well be applied to the high temperature insulating field;
(2) come the pore structure of final foam materials is controlled through the design and the proportioning of composite pore-forming agent; Can guarantee the stable of porous insert pore structure and do not subside; Through follow-up sintering process, the TiAl intermetallic compound porous material that is preparation can obtain high porosity possessing under the prerequisite of certain structural strength; And the technological process simple controllable helps large-scale production;
(3) prepared foam TiAl intermetallic compound steady quality has good repeatability.
Embodiment
Embodiment 1
Get 80% Ti element powders, 20% Al element powders mixing by mass ratio; Wherein: Ti powder degree is 300～400 orders; Al powder degree is 200～300 orders; Mixed powder TV by Ti Al powder and pore-forming material is 100%, adds bicarbonate of ammonia, the urea that accounts for mixed powder TV 10% that accounts for mixed powder TV 25%, the lime carbonate that accounts for mixed powder TV 5%; Ball mill mixing, ball-to-powder weight ratio are 8: 1, and mixing time is 4h.Adopt the press moulding mode press forming, obtain the mold pressing base; Pressing pressure is 200MPa; Place vacuum tightness 1.0 * 10 the mold pressing base
-1In the process furnace of Pa, be heated to 80 ℃ with 5 ℃/min heat-up rate, insulation 30min hangs down the thermophase degreasing; Then, be heated to 200 ℃, insulation 80min, thermophase degreasing in carrying out with 5 ℃/min heat-up rate; At last, be heated to 1000 ℃ with 2 ℃/min heat-up rate, insulation 60min carries out the hot stage degreasing.Degreasing is heated to 1300 ℃ with 10 ℃/min heat-up rate after accomplishing, and insulation 120min carries out vacuum sintering.Making porosity is 80%, and ultimate compression strength is the foam TiAl inter-metallic compound material of 2.2MPa.
Embodiment 2
Get 60% Ti element powders, 40% Al element powders mixing by mass ratio; Wherein: Ti powder degree is 200～325 orders; Al powder degree is 325～400 orders; Mixed powder TV by Ti Al powder and pore-forming material is 100%, adds volatile salt, the Zinic stearas that accounts for mixed powder TV 30% that accounts for mixed powder TV 20%, the lime carbonate that accounts for mixed powder TV 30%; Ball mill mixing, ball-to-powder weight ratio are 10: 1, and mixing time is 6h.Adopt isostatic cool pressing mode press forming, obtain pressed compact; Pressing pressure is 300MPa; Place vacuum tightness 1.0 * 10 pressed compact
-2In the process furnace of Pa, be heated to 60 ℃ with 9 ℃/min heat-up rate, insulation 60min hangs down the thermophase degreasing; Then, be heated to 340 ℃, insulation 60min, thermophase degreasing in carrying out with 2 ℃/min heat-up rate; At last, be heated to 840 ℃ with 5 ℃/min heat-up rate, insulation 90min carries out the hot stage degreasing.Degreasing is heated to 1200 ℃ with 13 ℃/min heat-up rate after accomplishing, and insulation 150min carries out vacuum sintering.Making porosity is 85%, and ultimate compression strength is the foam TiAl inter-metallic compound material of 1.9MPa.
Embodiment 3
Get 50% Ti element powders, 50% Al element powders mixing by mass ratio; Wherein: Ti powder degree is 100～200 orders; Al powder degree is 200～325 orders; Mixed powder TV by Ti Al powder and pore-forming material is 100%, adds bicarbonate of ammonia, the Zinic stearas that accounts for mixed powder TV 25% that accounts for mixed powder TV 15%, the magnesiumcarbonate that accounts for mixed powder TV 35%; Ball mill mixing, ball-to-powder weight ratio are 6: 1, and mixing time is 8h.Adopt isostatic cool pressing mode press forming, obtain pressed compact; Pressing pressure is 50MPa; Place vacuum tightness 1.0 * 10 pressed compact
-3In the process furnace of Pa, be heated to 70 ℃ with 6 ℃/min heat-up rate, insulation 90min hangs down the thermophase degreasing; Then, be heated to 180 ℃, insulation 120min, thermophase degreasing in carrying out with 8 ℃/min heat-up rate; At last, be heated to 800 ℃ with 3 ℃/min heat-up rate, insulation 60min carries out the hot stage degreasing.Degreasing is heated to 1350 ℃ with 15 ℃/min heat-up rate after accomplishing, and insulation 180min carries out vacuum sintering.Making porosity is 88%, and ultimate compression strength is the foam TiAl inter-metallic compound material of 1.7MPa.
Embodiment 4
Get 40% Ti element powders, 60% Al element powders mixing by mass ratio; Wherein: Ti powder degree is 100～300 orders; Al powder degree is 200～400 orders; Mixed powder TV by Ti Al powder and pore-forming material is 100%, adds volatile salt, the urea that accounts for mixed powder TV 40% that accounts for mixed powder TV 35%, the magnesiumcarbonate that accounts for mixed powder TV 15%; Ball mill mixing, ball-to-powder weight ratio are 2: 1, and mixing time is 12h.Adopt the press moulding mode press forming, obtain pressed compact; Pressing pressure is 400MPa; Place vacuum tightness 1.0 * 10 pressed compact
-2In the process furnace of Pa, be heated to 50 ℃ with 7 ℃/min heat-up rate, insulation 120min hangs down the thermophase degreasing; Then, be heated to 150 ℃, insulation 120min, thermophase degreasing in carrying out with 10 ℃/min heat-up rate; At last, be heated to 550 ℃ with 6 ℃/min heat-up rate, insulation 120min carries out the hot stage degreasing.Degreasing is heated to 1400 ℃ with 20 ℃/min heat-up rate after accomplishing, and insulation 120min carries out vacuum sintering.Making porosity is 90%, and ultimate compression strength is the foam TiAl inter-metallic compound material of 1.5MPa.
Claims (3)
1. the preparation method of a foam TiAl intermetallic compound comprises the steps:
The first step: getting granularity is 100～400 purpose Ti powder, Al powder, is the Ti powder by mass percentage: Al powder=(40～80): mix (20～60); Mixed powder TV by Ti Al powder and pore-forming material is 100%, adds the low-temperature decomposition temperature pore-forming material that accounts for mixed powder TV 15%～35%; Add the middle temperature decomposition temperature pore-forming material that accounts for mixed powder TV 10%～40%; Add the high-temperature decomposition temperature pore-forming material that accounts for mixed powder TV 5%～35%; Ball mill mixing is even; Obtain the mixture of Ti powder, Al powder and pore-forming material; Said low-temperature decomposition temperature pore-forming material is selected from least a in bicarbonate of ammonia, the volatile salt; Warm decomposition temperature pore-forming material is selected from least a in urea, the Zinic stearas in said; The high-temperature decomposition temperature pore-forming material is selected from least a in lime carbonate, the magnesiumcarbonate;
Second step: with the first step gained mixture compression moulding post-heating, vacuum tightness is 1.0 * 10 in the control stove
-1～1.0 * 10
-3Pa is incubated respectively by low thermophase, middle thermophase, hot stage, removes low-temperature decomposition temperature pore-forming material, middle temperature decomposition temperature pore-forming material, high-temperature decomposition temperature pore-forming material successively; Obtain the TiAl powder mold pressing base of high porosity; Then, be heated to sintering temperature and carry out sintering, the porosity that promptly obtains having certain intensity is up to the foam TiAl inter-metallic compound material more than 80%; The heating cycle of sintering process is: 10～20 ℃/min of rate of heating, 1200～1400 ℃ of sintering temperatures, soaking time 120～180min; Said low thermophase heating cycle is: 5～10 ℃/min of rate of heating, 50～100 ℃ of holding temperatures, soaking time 30～120min; The thermophase heating cycle is in said: 2～10 ℃/min of rate of heating, 150～350 ℃ of holding temperatures, soaking time 60～120min; Said hot stage heating cycle is: 2～5 ℃/min of rate of heating, 500～1000 ℃ of holding temperatures, soaking time 60～120min.
2. the preparation method of a kind of foam TiAl intermetallic compound according to claim 1 is characterized in that: the ball-to-powder weight ratio of said ball mill mixing is (2～10): 1, and mixing time 4h～12h.
3. the preparation method of a kind of foam TiAl intermetallic compound according to claim 1 and 2 is characterized in that: a kind of in isostatic cool pressing, the mold pressing adopted in said compression moulding, and pressing pressure is 50MPa～400MPa.
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| CN102786314B (en) * | 2012-08-23 | 2014-01-01 | 武汉钢铁(集团)公司 | Fused-rebonded magnesite-chrome brick with excellent thermal shock resistance and production process |
| CN102864323B (en) * | 2012-09-25 | 2014-07-02 | 中国科学院金属研究所 | Preparation method of Ni-Al alloy porous material with controllable structure |
| CN104070164B (en) * | 2014-07-16 | 2016-08-24 | 哈尔滨工业大学 | The method of powder sintered synthesizing porous Intermatallic Ti-Al compound |
| CN105200281B (en) * | 2015-10-19 | 2017-03-29 | 湘潭大学 | A kind of Al Mg alloy porous materials and preparation method thereof |
| CN105506330B (en) * | 2015-12-10 | 2017-11-24 | 中国兵器科学研究院宁波分院 | Microwave liquid-phase sintering process composite porous high temperature resistant TiAl |
| CN106399741A (en) * | 2016-10-02 | 2017-02-15 | 桂林理工大学 | Method for sintering and preparing 7-series foam aluminum alloy material through pore-forming agent method |
| CN106381413A (en) * | 2016-10-02 | 2017-02-08 | 桂林理工大学 | Method for preparing 5-series foam aluminum alloy material through pore forming agent method |
| CN106893898B (en) * | 2017-03-08 | 2018-12-14 | 湖南云平环保科技有限公司 | Porous material supporter and preparation method thereof between FeAl metal |
| CN107790722A (en) * | 2017-10-31 | 2018-03-13 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of preparation method of double-pore structure TiAl porous materials |
| CN109108843A (en) * | 2018-08-23 | 2019-01-01 | 沈阳中科超硬磨具磨削研究所 | A kind of vitrified abrasive |
| CN110777275A (en) * | 2019-10-10 | 2020-02-11 | 太原理工大学 | Titanium-aluminum three-dimensional through hole structure material and preparation method thereof |
| CN112170845B (en) * | 2020-09-28 | 2022-09-20 | 西部宝德科技股份有限公司 | Degreasing method for powder porous metal film |
| CN115247238B (en) * | 2021-12-10 | 2023-10-13 | 榆林学院 | Al-Ti intermetallic compound porous material based on synergistic pore-forming mechanism and preparation method thereof |
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| CN1314477C (en) * | 2004-01-13 | 2007-05-09 | 中南大学 | Method for preparing titanium-aluminum intermetallic compound filter membrane by reacting and synthesizing titanium and aluminum element powder |
| CN100557050C (en) * | 2008-04-24 | 2009-11-04 | 中南大学 | A kind of preparation method of nickel-aluminum base alloy porous material |
| CN101358304B (en) * | 2008-09-27 | 2010-12-08 | 成都易态科技有限公司 | Nial intermetallic compound porous material and preparation method thereof |
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