CN108504901A - A kind of preparation method of titanium nickel cobalt memorial alloy body - Google Patents
A kind of preparation method of titanium nickel cobalt memorial alloy body Download PDFInfo
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- CN108504901A CN108504901A CN201810285186.8A CN201810285186A CN108504901A CN 108504901 A CN108504901 A CN 108504901A CN 201810285186 A CN201810285186 A CN 201810285186A CN 108504901 A CN108504901 A CN 108504901A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
- B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
- B22F3/1134—Inorganic fillers
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/007—Alloys based on nickel or cobalt with a light metal (alkali metal Li, Na, K, Rb, Cs; earth alkali metal Be, Mg, Ca, Sr, Ba, Al Ga, Ge, Ti) or B, Si, Zr, Hf, Sc, Y, lanthanides, actinides, as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/006—Resulting in heat recoverable alloys with a memory effect
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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Abstract
The invention discloses a kind of preparation methods of titanium nickel cobalt memorial alloy body, the method overcome uncontrollable and alloy product the damping capacity of porosity and aperture in existing porous TiNiCo marmems preparation method and pass and other mechanical properties, it is still necessary to the defects of raising, the TiNiCo marmems of this method processing, its internal grain size is sub-micrometer scale, tiny crystallite dimension can strengthen TiNiCo shape memory alloy bases with precipitated phase, to reduce the temperature that R phase transition is martensitic phase, temperature range existing for R phases is caused to expand.This improves the recovery characters of alloy further to provide convenience condition using R phase transformations, improves the cyclical stability of alloy.
Description
Technical field
The present invention relates to alloy material manufacturing fields, and in particular to a kind of preparation method of titanium nickel cobalt memorial alloy body.
Background technology
Marmem（Shape Memory Alloy, SMA）Refer to after suitably deforming, in certain physical condition
Change the alloy for descending energy automatic working and restoring shape before deforming.Marmem is because it is with higher restorability shape
Become, it has also become a kind of important functional material is applied widely.NiTi system shape memory has reminiscence original shape, nothing
Magnetism, wear-and corrosion-resistant, high temperature resistant, avirulent feature.But, the yield strength of current marmem generally exists
700MPa or less.
Memorial alloy is usually used in the surgical implants such as human synovial, for it is compared to stainless steel and titanium alloy, mechanicalness
Higher wearability can be possessed closer to the mechanical performance of cortex of bone.But it is negative that the low-corrosiveness of this material brings some
Face is rung, and the corrosion products that alloy surface generates cause cytotoxicity to increase, and make cell unusual death.However these materials
Micro-structure and surface morphology homogeneity can be changed memorial alloy corrosion resistance and wear resistance.
TiNi base marmems have abundant martensitic traoformation phenomenon, excellent recovery characters and biology
Compatibility, damping characteristic etc., therefore obtain extensive use in fields such as aerospace, mechano-electronic, biologic medicals.TiNi bases close
The good characteristic of gold is mostly from the transformation behavior between its parent phase and martensitic phase.The martensitic traoformation product of TiNi based alloys
It is more, include the R phases of the B19 martensitic phases of the B19 ' martensitic phases of monocline, orthohormbic structure and water chestnut square structure.With other two
Kind martensitic traoformation compares, and the transformation between B2 parent phases and R phases has lot of advantages, such as thermo-lag small (being no more than 5 DEG C), cycle
Stability is good, damping loss factor is high, response frequency is high etc..
Invention content
The present invention provides a kind of preparation method of titanium nickel cobalt memorial alloy body, and the method overcome existing porous TiNiCo
In marmem preparation method porosity and aperture and pass be difficult to control and the damping capacity of alloy product and its
It is still necessary to the defects of raising for his mechanical property, and the TiNiCo marmems of this method processing, internal grain size is sub-micro
Rice magnitude, tiny crystallite dimension can strengthen TiNiCo shape memory alloy bases with precipitated phase, be horse to reduce R phase transition
The temperature of family name's body phase causes temperature range existing for R phases to expand.This is further provides convenience condition using R phase transformations, simultaneously
The recovery characters for improving alloy, improve the cyclical stability of alloy.
To achieve the goals above, the present invention provides a kind of preparation method of titanium nickel cobalt memorial alloy body, this method packets
Include following steps：
（1）Dispensing
Mixed powder is prepared by following parts by weight
25-28 parts of titanium valve；
42-45 parts of nickel powder；
12-16 parts of cobalt powder
0.5-1.5 parts of yttrium powder
Mixed powder is placed in stainless steel jar mill, is sealed after filling absolute ethyl alcohol, the ball milling 3-4h on planetary ball mill, ball
For the ratio of grinding media to material used in mill for 10: 1, the rotating speed of ball mill is 400-500r/min, and later, the good mixed powder of ball milling is taken out simultaneously
It is placed on filter paper and stands 6-8 minutes, obtain raw material powder；
（2）Prepare memorial alloy matrix
Above-mentioned raw materials powder is uniformly mixed with the water KCl particles that decrystallize, and the dosage for the water KCl particles that decrystallize accounts for mixed powder and go for it
The 65-75% of the percent by volume of crystallization water KCl granulate mixtures, fills after which is mixed 45-50min in batch mixer
In the stainless steel mould for entering inner wall coating zinc stearate, green compact are made in the unidirectional 380-400MPa that pressurizes, and are later packed into the green compact
Alumina crucible is placed in tube type vacuum sintering furnace, after vacuum is evacuated to 1-5Pa in stove, is added with the rate of 5-10 DEG C/min
Heat is to 800-810 DEG C, after keeping the temperature 3-4h, then with 10-15 DEG C/min of rate is heated to 960-980 DEG C, keeps the temperature after 3-4h with stove
It is cooled to room temperature, sintered body is taken out out of stove, be placed in ultrasound bath after cleaning 15-20min and dry, porous alloy is made
Matrix；
（3）Memorial alloy matrix is obtained into crystallite dimension between the alloy of 200-250nm, subsequent anneal temperatures by subsequent anneal
It is 450-550 DEG C, soaking time 30-45min；Ultra-fine Grained memorial alloy matrix is prepared using Equal Channel Angular Pressing processing, specifically
Extrusion process is as follows：Path Bc is squeezed, passage 9-11 is squeezed, squeezes 480-500 DEG C of temperature, extrusion die interior angle is 120 °；
Above-mentioned memorial alloy matrix is placed in vacuum heat treatment furnace, is evacuated to 1 × 10-3-1×10-4Pa is 250- in temperature
Ageing treatment 15-20h under the conditions of 350 DEG C；
The memorial alloy matrix of ageing treatment is removed into surface scale, you can obtain there is wider R phases that there are temperature ranges
Titanium nickel cobalt memorial alloy body.
The present invention has following advantages：
（1）Porosity and aperture and pass in existing porous TiNiCo marmems preparation method is overcome to be difficult to control
It is still necessary to the defects of raising for the damping capacity and other mechanical properties of system and alloy product；
（2）The TiNiCo marmems of this method processing, internal grain size are sub-micrometer scale, tiny crystal grain ruler
It is very little to strengthen TiNiCo shape memory alloy bases with precipitated phase, to reduce the temperature that R phase transition is martensitic phase, cause R
Temperature range existing for phase expands.This is further provides convenience condition using R phase transformations, while the shape for improving alloy is restored
Characteristic improves the cyclical stability of alloy.
Specific implementation mode
Embodiment one
Mixed powder is prepared by following parts by weight
25 parts of titanium valve；
42 parts of nickel powder；
12 parts of cobalt powder
0.5 part of yttrium powder
Mixed powder is placed in stainless steel jar mill, is sealed after filling absolute ethyl alcohol, the ball milling 3h on planetary ball mill, ball milling
For the middle ratio of grinding media to material used for 10: 1, the rotating speed of ball mill is 400r/min, later, the good mixed powder taking-up of ball milling is placed in filter
6 minutes are stood on paper, obtains raw material powder.
Above-mentioned raw materials powder is uniformly mixed with the water KCl particles that decrystallize, and the dosage for the water KCl particles that decrystallize accounts for mixed powder for it
With the 65% of the percent by volume for the water KCl granulate mixtures that decrystallize, it is packed into after which is mixed 45min in batch mixer
Inner wall coats in the stainless steel mould of zinc stearate, and green compact are made in the unidirectional 380MPa that pressurizes, and the green compact are packed into aluminium oxide later
Crucible is placed in tube type vacuum sintering furnace, after vacuum is evacuated to 1Pa in stove, is heated to 800 DEG C with the rate of 5 DEG C/min, is protected
It after warm 3h, then with 10 DEG C/min of rate is heated to 960 DEG C, cools to room temperature with the furnace after keeping the temperature 3h, sintered body is taken out of stove
Go out, be placed in ultrasound bath after cleaning 15min and dry, porous alloy matrix is made.
Memorial alloy matrix is obtained into crystallite dimension between the alloy of 200-250nm, subsequent anneal temperature by subsequent anneal
Degree is 450-550 DEG C, soaking time 30-45min；Ultra-fine Grained memorial alloy matrix is prepared using Equal Channel Angular Pressing processing, is had
Body extrusion process is as follows：Path Bc is squeezed, passage 9-11 is squeezed, squeezes 480-500 DEG C of temperature, extrusion die interior angle is 120 °.
Above-mentioned memorial alloy matrix is placed in vacuum heat treatment furnace, is evacuated to 1 × 10-3-1×10-4Pa is in temperature
Ageing treatment 15-20h under the conditions of 250-350 DEG C；The memorial alloy matrix of ageing treatment is removed into surface scale, you can obtain
With wider R phases, there are the titanium nickel cobalt memorial alloy bodies of temperature range.
Embodiment two
Mixed powder is prepared by following parts by weight
28 parts of titanium valve；
45 parts of nickel powder；
16 parts of cobalt powder
1.5 parts of yttrium powder
Mixed powder is placed in stainless steel jar mill, is sealed after filling absolute ethyl alcohol, the ball milling 3-4h on planetary ball mill, ball
For the ratio of grinding media to material used in mill for 10: 1, the rotating speed of ball mill is 400-500r/min, and later, the good mixed powder of ball milling is taken out simultaneously
It is placed on filter paper and stands 6-8 minutes, obtain raw material powder.
Above-mentioned raw materials powder is uniformly mixed with the water KCl particles that decrystallize, and the dosage for the water KCl particles that decrystallize accounts for mixed powder for it
With the 75% of the percent by volume for the water KCl granulate mixtures that decrystallize, it is packed into after which is mixed 50min in batch mixer
Inner wall coats in the stainless steel mould of zinc stearate, and green compact are made in the unidirectional 400MPa that pressurizes, and the green compact are packed into aluminium oxide later
Crucible is placed in tube type vacuum sintering furnace, and after vacuum is evacuated to 5Pa in stove, 810 DEG C are heated to the rate of 10 DEG C/min,
It after keeping the temperature 4h, then with 15 DEG C/min of rate is heated to 980 DEG C, room temperature is cooled to the furnace after keeping the temperature 4h, by sintered body out of stove
It takes out, is placed in ultrasound bath after cleaning 20min and dries, porous alloy matrix is made.
Memorial alloy matrix is obtained into crystallite dimension between the alloy of 200-250nm, subsequent anneal temperature by subsequent anneal
Degree is 450-550 DEG C, soaking time 30-45min；Ultra-fine Grained memorial alloy matrix is prepared using Equal Channel Angular Pressing processing, is had
Body extrusion process is as follows：Path Bc is squeezed, passage 9-11 is squeezed, squeezes 480-500 DEG C of temperature, extrusion die interior angle is 120 °.
Above-mentioned memorial alloy matrix is placed in vacuum heat treatment furnace, is evacuated to 1 × 10-3-1×10-4Pa is in temperature
Ageing treatment 15-20h under the conditions of 250-350 DEG C；The memorial alloy matrix of ageing treatment is removed into surface scale, you can obtain
With wider R phases, there are the titanium nickel cobalt memorial alloy bodies of temperature range.
Claims (1)
1. a kind of preparation method of titanium nickel cobalt memorial alloy body, this method comprises the following steps：
（1）Dispensing
Mixed powder is prepared by following parts by weight
25-28 parts of titanium valve；
42-45 parts of nickel powder；
12-16 parts of cobalt powder
0.5-1.5 parts of yttrium powder
Mixed powder is placed in stainless steel jar mill, is sealed after filling absolute ethyl alcohol, the ball milling 3-4h on planetary ball mill, ball
For the ratio of grinding media to material used in mill for 10: 1, the rotating speed of ball mill is 400-500r/min, and later, the good mixed powder of ball milling is taken out simultaneously
It is placed on filter paper and stands 6-8 minutes, obtain raw material powder；
（2）Prepare memorial alloy matrix
Above-mentioned raw materials powder is uniformly mixed with the water KCl particles that decrystallize, and the dosage for the water KCl particles that decrystallize accounts for mixed powder and go for it
The 65-75% of the percent by volume of crystallization water KCl granulate mixtures, fills after which is mixed 45-50min in batch mixer
In the stainless steel mould for entering inner wall coating zinc stearate, green compact are made in the unidirectional 380-400MPa that pressurizes, and are later packed into the green compact
Alumina crucible is placed in tube type vacuum sintering furnace, after vacuum is evacuated to 1-5Pa in stove, is added with the rate of 5-10 DEG C/min
Heat is to 800-810 DEG C, after keeping the temperature 3-4h, then with 10-15 DEG C/min of rate is heated to 960-980 DEG C, keeps the temperature after 3-4h with stove
It is cooled to room temperature, sintered body is taken out out of stove, be placed in ultrasound bath after cleaning 15-20min and dry, porous alloy is made
Matrix；
（3）Memorial alloy matrix is obtained into crystallite dimension between the alloy of 200-250nm, subsequent anneal temperatures by subsequent anneal
It is 450-550 DEG C, soaking time 30-45min；Ultra-fine Grained memorial alloy matrix is prepared using Equal Channel Angular Pressing processing, specifically
Extrusion process is as follows：Path Bc is squeezed, passage 9-11 is squeezed, squeezes 480-500 DEG C of temperature, extrusion die interior angle is 120 °；
Above-mentioned memorial alloy matrix is placed in vacuum heat treatment furnace, is evacuated to 1 × 10-3-1×10-4Pa is 250- in temperature
Ageing treatment 15-20h under the conditions of 350 DEG C；
The memorial alloy matrix of ageing treatment is removed into surface scale, you can obtain there is wider R phases that there are temperature ranges
Titanium nickel cobalt memorial alloy body.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810285186.8A CN108504901A (en) | 2018-04-02 | 2018-04-02 | A kind of preparation method of titanium nickel cobalt memorial alloy body |
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| CN201810285186.8A CN108504901A (en) | 2018-04-02 | 2018-04-02 | A kind of preparation method of titanium nickel cobalt memorial alloy body |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113166854A (en) * | 2020-06-08 | 2021-07-23 | 南京江东工贸有限公司 | Metal material and preparation method and application thereof |
| CN114512823A (en) * | 2022-01-12 | 2022-05-17 | 中国电子科技集团公司第十研究所 | Self-adaptive packaging process method for large-scale array elements of phased-array antenna |
Citations (5)
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|---|---|---|---|---|
| CN102031405A (en) * | 2010-12-09 | 2011-04-27 | 河北工业大学 | Preparation method of porous CuAlMn shape memory alloy |
| CN106282812A (en) * | 2015-06-02 | 2017-01-04 | 上海交通大学 | A kind of shape memory alloy material and the application on pipe joint thereof |
| CN107008905A (en) * | 2017-02-25 | 2017-08-04 | 河北工业大学 | The preparation method of TiNiCu marmem based damping composite materials |
| CN107043867A (en) * | 2017-01-09 | 2017-08-15 | 河北工业大学 | A kind of preparation method of porous copper-based shape memory alloy |
| CN107475652A (en) * | 2017-08-22 | 2017-12-15 | 哈尔滨工程大学 | In a kind of regulation and control TiNi base memorial alloys there is the method in section in R phases |
-
2018
- 2018-04-02 CN CN201810285186.8A patent/CN108504901A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102031405A (en) * | 2010-12-09 | 2011-04-27 | 河北工业大学 | Preparation method of porous CuAlMn shape memory alloy |
| CN106282812A (en) * | 2015-06-02 | 2017-01-04 | 上海交通大学 | A kind of shape memory alloy material and the application on pipe joint thereof |
| CN107043867A (en) * | 2017-01-09 | 2017-08-15 | 河北工业大学 | A kind of preparation method of porous copper-based shape memory alloy |
| CN107008905A (en) * | 2017-02-25 | 2017-08-04 | 河北工业大学 | The preparation method of TiNiCu marmem based damping composite materials |
| CN107475652A (en) * | 2017-08-22 | 2017-12-15 | 哈尔滨工程大学 | In a kind of regulation and control TiNi base memorial alloys there is the method in section in R phases |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113166854A (en) * | 2020-06-08 | 2021-07-23 | 南京江东工贸有限公司 | Metal material and preparation method and application thereof |
| CN114512823A (en) * | 2022-01-12 | 2022-05-17 | 中国电子科技集团公司第十研究所 | Self-adaptive packaging process method for large-scale array elements of phased-array antenna |
| CN114512823B (en) * | 2022-01-12 | 2023-09-01 | 中国电子科技集团公司第十研究所 | Phased array antenna array surface array element self-adaptive packaging process method |
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