CN111172484A - Laser selective melting cobalt-chromium alloy false tooth infrared heating annealing heat treatment method - Google Patents
Laser selective melting cobalt-chromium alloy false tooth infrared heating annealing heat treatment method Download PDFInfo
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- CN111172484A CN111172484A CN202010046481.5A CN202010046481A CN111172484A CN 111172484 A CN111172484 A CN 111172484A CN 202010046481 A CN202010046481 A CN 202010046481A CN 111172484 A CN111172484 A CN 111172484A
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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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- 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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/045—Cobalt or cobalt alloys
-
- 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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
-
- 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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/30—Process control
- B22F10/36—Process control of energy beam parameters
-
- 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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/30—Process control
- B22F10/37—Process control of powder bed aspects, e.g. density
-
- 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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/60—Treatment of workpieces or articles after build-up
- B22F10/64—Treatment of workpieces or articles after build-up by thermal means
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
-
- 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
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/12—Materials or treatment for tissue regeneration for dental implants or prostheses
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention discloses an infrared heating annealing heat treatment method for melting a cobalt-chromium alloy false tooth by selective laser, belonging to the technical field of heat treatment. The cobalt-chromium alloy false tooth formed by melting through laser selection is placed in a tubular infrared heating furnace, annealing heat treatment is carried out on the cobalt-chromium alloy false tooth by adopting infrared heating, the heat preservation temperature of the infrared heating annealing heat treatment is 850-1050 ℃, the heat preservation time is 5-25min, the cobalt-chromium alloy false tooth is firstly cooled to 300 ℃ along with the furnace, and then the cobalt-chromium alloy false tooth is taken out and air-cooled to room temperature. Compared with the mode of heating the cobalt-chromium alloy false tooth by using a resistance wire through convection heat transfer, the infrared heating has the advantages of high heating speed, short heat preservation time and high heat treatment efficiency because the infrared heating is through radiation heat transfer.
Description
Technical Field
The invention relates to an infrared heating annealing heat treatment method for melting a cobalt-chromium alloy false tooth by selective laser, belonging to the technical field of heat treatment.
Background
Cobalt-chromium alloys have good mechanical properties and biocompatibility, and thus are widely used in the field of medical devices such as dentistry. Selective Laser Melting (SLM) is one of additive manufacturing techniques, where 3D data is sliced in layers by software, and then a high-energy laser beam melts the powder layer by layer to obtain a dense three-dimensional solid part. However, in the selective laser melting and forming process, the material is rapidly melted and solidified, the temperature gradient is large, and thermal stress is easily accumulated, so that the part is easy to deform. Therefore, annealing heat treatment needs to be performed on the workpiece subjected to selective laser melting forming to remove internal stress and prevent deformation.
In the prior art, the part is subjected to annealing heat treatment by adopting a resistance wire heating mode and a convection heat transfer mode, the heating rate is only 10-20 ℃/min generally, and the heat preservation time is about 2 hours, so that the problems of low heating rate, long heat preservation time and the like exist in the conventional resistance wire heating mode, and the heat treatment efficiency is low.
Disclosure of Invention
In view of the above problems, the present invention provides a method for annealing heat treatment by infrared heating, which is based on the principle that when the wavelength of infrared rays is consistent with the absorption wavelength of an object to be heated, the object to be heated absorbs a large amount of infrared rays, and molecules and atoms in the object resonate and generate strong vibration and rotation, so that the temperature of the object to be heated is raised, and the object to be heated is heated. Compared with the conventional resistance wire for heating the cobalt-chromium alloy false tooth in a convection heat transfer mode, the infrared heating device has the advantages of high heating speed, short heat preservation time and high heat treatment efficiency because the infrared heating is carried out through radiation heat transfer.
The invention aims to provide a heat treatment method for a selective laser melting material, which comprises the steps of putting the selective laser melting material into a tubular infrared heating furnace, and carrying out annealing heat treatment on the selective laser melting material by adopting infrared heating.
In one embodiment of the present invention, the selective laser melting material is cobalt-chromium alloy.
In one embodiment of the present invention, the process parameters of selective laser melting are as follows: the laser power is 200-300W, the spot diameter is 0.02-0.05mm, the scanning speed is 600-800mm/s, and the powder layer thickness is 0.02-0.04 mm.
In one embodiment of the present invention, the process parameters of the infrared heating annealing heat treatment are as follows: the far infrared wavelength is 2.5-15 mu m; the highest temperature is 850-1050 ℃, and the heat preservation time is 5-25 min.
Preferably, the maximum temperature is 950-1000 deg.C, and the holding time is 10-15 min.
In one embodiment of the present invention, the infrared heating annealing heat treatment comprises the following specific process steps:
(1) placing the cobalt-chromium alloy false tooth which is melted and formed by laser selection into a tubular infrared heating furnace, and vacuumizing;
(2) and (3) heating: heating from room temperature to 850-1050 deg.C at a heating rate of 50-150 deg.C/min;
(3) and (3) heat preservation: keeping the temperature at 850-1050 deg.C for 5-25 min;
(4) and (6) cooling.
In one embodiment of the present invention, the cooling mode is one or both of air cooling and furnace cooling.
In one embodiment of the invention, the furnace cooling and air cooling combined cooling is carried out after furnace cooling to 200-300 ℃ and then air cooling to room temperature.
The second purpose of the invention is to provide a selective laser melting material prepared by the method.
The third purpose of the invention is to provide the application of the selective laser melting material in preparing the dental prosthesis.
The invention has the beneficial effects that:
the principle of infrared heating is that when the wavelength of infrared ray is consistent with the absorption wavelength of the heated object, the heated object absorbs a large amount of far infrared ray, and at the moment, molecules and atoms in the object resonate and generate strong vibration and rotation, so that the temperature of the object is raised, and the purpose of heating is achieved. Compared with the mode of heating the cobalt-chromium alloy false tooth by using a resistance wire through convection heat transfer, the infrared heating has the advantages of high heating speed, short heat preservation time and high heat treatment efficiency because the infrared heating is through radiation heat transfer. The cobalt-chromium alloy false tooth after heat treatment by the process has the advantages of complete internal stress removal, no deformation, improvement of the strength and toughness of the false tooth and improvement of the comprehensive mechanical property of the material.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.
The internal stress testing method comprises the following steps: according to the experiment of melting metal materials in laser selective area for fixed and movable restoration of oral cavity by dental additive manufacturing, see concretelyhttps://max.book118.com/html/2018/1209/ 5332312303001334.shtm。
Example 1:
an infrared heating annealing heat treatment method for a cobalt-chromium alloy false tooth formed by selective laser melting is characterized in that the cobalt-chromium alloy false tooth is formed by selective laser melting according to technological parameters recommended by a 3D printer manufacturer, and the chemical components of cobalt-chromium alloy powder and the technological parameters selected by selective laser melting are shown in tables 1 and 2 respectively.
The cobalt-chromium alloy false tooth which is melted and formed by laser selective area is subjected to stress relieving annealing in vacuum, and the method comprises the following steps:
the cobalt-chromium alloy false tooth formed by melting through laser selective area is put into a tubular infrared heating furnace, vacuumized to-0.01 MPa, and then subjected to infrared heating annealing heat treatment, and the specific process comprises the following steps:
(1) raising the temperature of the cobalt-chromium alloy denture from room temperature to 950 ℃ at 100 ℃/min;
(2) keeping the temperature at 950 ℃ for 15 min;
(3) stopping heating, cooling to 300 ℃ along with the furnace, taking out from the furnace, and air cooling.
The internal stress of the cobalt-chromium alloy false tooth treated by the process is completely removed without deformation. Meanwhile, the strength and the toughness of the false tooth are improved, and the comprehensive mechanical property of the material is improved.
TABLE 1 chemical composition of Co-Cr alloy (mass fraction,%)
TABLE 2 Selective laser melting Process parameters
Example 2: influence of maximum temperature on deformation
The effect of the stress relief annealing heat treatment of the cobalt-chromium alloy is closely related to the process parameters such as the highest heating temperature, the heat preservation time, the cooling mode and the like.
Compared with the example 1, the method is characterized in that the warping sample of the cobalt-chromium alloy is heated to 850 ℃, 900 ℃, 950 ℃, 1000 ℃ and 1050 ℃ from the room temperature by 100 ℃/min and is kept warm for 15min, and is taken out along with the cooling of the furnace to the room temperature after the completion, the warping sample is separated from the substrate by wire cutting, the deformation of the warping sample is measured by a vernier caliper, and the heat treatment effect is observed, and the specific experimental scheme is shown in the table 3.
TABLE 3 protocol for varying the maximum temperature
As is clear from Table 3, the deformation amount of the warp specimens in experiment 1 was 0.12mm, the deformation amount of the warp specimens in experiment 2 was 0.05mm, and the deformation amounts of the warp specimens in experiments 3, 4, and 5 were all 0. In experiment 1, the maximum heating temperature is low, and the internal stress in the cobalt-chromium alloy is not completely eliminated, so that the deformation of the warped sample is large. By raising the maximum temperature appropriately to 900 ℃, the residual stress of the warped sample in experiment 2 was reduced, resulting in only slight distortion. When the maximum temperature was increased to 950 ℃, the amount of deformation of the warped sample in experiment 3 was reduced to 0. However, as the maximum temperature further increased to 1000 ℃, the cobalt chromium alloy grains began to grow and the mechanical properties decreased in experiment 4. When the maximum temperature reached 1050 ℃, the cobalt chromium alloy grains became coarse in experiment 5, resulting in a significant decrease in mechanical properties.
Through the experiment of the influence of the maximum temperature on the deformation of the cobalt-chromium alloy warping sample, the research finds that the suitable maximum heating temperature is 950 ℃.
Example 3: influence of holding time on deformation
Compared with the example 1, the method is characterized in that the temperature of a cobalt-chromium alloy warping sample is increased to 950 ℃ from room temperature at a speed of 100 ℃/min, the temperature is respectively maintained for 5min, 10min, 15min, 20min and 25min, the sample is taken out along with cooling of a furnace to room temperature after the temperature is up, the warping sample is separated from a substrate through wire cutting, the deformation of the warping sample is measured by a vernier caliper, and the heat treatment effect is observed, wherein the specific experimental scheme is shown in table 4.
TABLE 4 protocol for varying incubation times
As is clear from Table 4, the deformation amount of the warp specimens in experiment a was 0.26mm, the deformation amount of the warp specimens in experiment b was 0.07mm, and the deformation amounts of the warp specimens in experiments c, d, and e were all 0.
In the experiment a, the internal stress of the warping sample is not completely eliminated due to the short heat preservation time, so the deformation amount is large. When the holding time was increased to 10min, the residual stress inside the warped sample in experiment b was small and only slight deformation occurred. The holding time is continued to be increased to 15min, and the warping sample is not deformed in the experiment c. When the holding time was increased to 20min, the warped sample did not deform in experiment d, but the grains started to grow. When the holding time was increased to 25min, the warped sample was not deformed in experiment e, but the crystal grains became coarse.
Through the experiment of the influence of the heat preservation time on the deformation of the cobalt-chromium alloy warping sample, the research finds that the suitable heat preservation time is 15 min.
Through multiple experiments, the warping sample is not deformed and the crystal grains are not basically grown when the maximum temperature is 950-1000 ℃ and the holding time is 10-15 min.
Example 4: influence of cooling mode on deformation
Compared with the example 1, the method is characterized in that the temperature of a cobalt-chromium alloy warping sample is raised to 950 ℃ from room temperature at a speed of 100 ℃/min, and the temperature is kept for 15min, in the first experiment, the warping sample is directly taken out from a furnace and air-cooled to the room temperature, in the second experiment, the warping sample is furnace-cooled to the room temperature, and in the third experiment, the warping sample is furnace-cooled to 300 ℃, and then is taken out and air-cooled to the room temperature. The warped sample was separated from the substrate by wire cutting, the amount of deformation of the warped sample was measured with a vernier caliper, and the heat treatment effect was observed, and the specific experimental protocol is shown in table 5.
TABLE 5 Experimental protocol for varying cooling regimes
As is clear from Table 5, the deformation amount of the warp specimens in the first experiment was 0.18mm, and the deformation amounts of the warp specimens in the second and third experiments were 0.
In the first experiment, the cooling speed is too high, so that the warping test piece generates stress again to cause deformation. In the second experiment, the cooling speed is slow by furnace cooling, the warping sample is not deformed, but the cooling time needs 180 min. Through multiple improvements, the sample is firstly cooled to 300 ℃ along with the furnace, then taken out and air-cooled to room temperature, the warping sample is not deformed, the cooling time is only 60min, and the cooling time is obviously shortened compared with the cooling time along with the furnace.
Through the experiment of the influence of the cooling mode on the deformation of the warping sample of the cobalt-chromium alloy, researches show that the suitable cooling mode is to cool the warping sample of the cobalt-chromium alloy to 300 ℃ along with the furnace, and then take out the warping sample of the cobalt-chromium alloy for air cooling to room temperature.
Comparative example 1:
the infrared heating in the embodiment 1 is replaced by resistance wire heating, and the specific process is as follows:
and putting the cobalt-chromium alloy warping sample into a box-type resistance furnace, and vacuumizing to-0.01 MPa. The method adopts a stress-relief annealing heat treatment process and comprises the following steps:
(1) the temperature was raised from room temperature to 450 ℃ for 60 min.
(2) And keeping the temperature for 45 min.
(3) The temperature rose to 750 ℃ in 45 min.
(4) And preserving the temperature for 60 min.
(5) Stopping heating, cooling to 300 ℃ along with the furnace, taking out from the furnace and air cooling.
Compared with infrared heating, the alloy is heated by the resistance wire, the alloy can be processed at a lower heating temperature and for a longer heat preservation time, the cobalt-chromium alloy is prevented from deforming, but the toughness of the false tooth after heat treatment is insufficient, and the requirement of clinical use cannot be completely met.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A heat treatment method for selective laser melting materials is characterized in that the selective laser melting materials are placed into a tubular infrared heating furnace, and annealing heat treatment is carried out on the selective laser melting materials by adopting infrared heating.
2. The method of claim 1 wherein the selective laser melting material is cobalt chromium.
3. The method according to claim 1 or 2, wherein the infrared thermal annealing heat treatment has process parameters of: the highest temperature is 850-1050 ℃, and the heat preservation time is 5-25 min.
4. The method according to any one of claims 1 to 3, wherein the infrared heating annealing heat treatment comprises the following specific process steps:
(1) placing the cobalt-chromium alloy false tooth which is melted and formed by laser selection into a tubular infrared heating furnace, and vacuumizing;
(2) and (3) heating: heating from room temperature to 850-1050 deg.C at a heating rate of 50-150 deg.C/min;
(3) and (3) heat preservation: keeping the temperature at 850-1050 deg.C for 5-25 min;
(4) and (6) cooling.
5. The method of claim 4, wherein the cooling is one or both of air cooling and furnace cooling.
6. The method of claim 5, wherein the combination of furnace cooling and air cooling is performed by cooling to 200-300 ℃ with the furnace and then cooling to room temperature.
7. The method according to any one of claims 1 to 6, wherein the infrared heating is performed by using far infrared rays having a wavelength of 2.5 to 15 μm.
8. The method according to any one of claims 1 to 7, wherein the process parameters of the selective laser melting molding are as follows: the laser power is 200-300W, the spot diameter is 0.02-0.05mm, the scanning speed is 600-800mm/s, and the powder layer thickness is 0.02-0.04 mm.
9. A selectively laser-melted material produced by the method of any one of claims 1 to 8.
10. Use of the selective laser melting material of claim 9 in the manufacture of a dental restoration.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11145530B2 (en) * | 2019-11-08 | 2021-10-12 | Cerebras Systems Inc. | System and method for alignment of an integrated circuit |
| CN113909497A (en) * | 2021-10-09 | 2022-01-11 | 江西金石三维智能制造科技有限公司 | Preparation method of selective laser melting cobalt-chromium alloy and cobalt-chromium denture alloy material |
| US11631600B2 (en) | 2017-08-24 | 2023-04-18 | Cerebras Systems Inc. | Apparatus and method for securing components of an integrated circuit |
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| DE102006056045A1 (en) * | 2006-11-28 | 2008-06-05 | Hausch, Gernot, Dr. | Cobalt-based dental alloy for production of ceramic-veneered crowns, bridges and other restorations, contains nickel, chromium, molybdenum, tungsten and cobalt, optionally with small amounts of other elements |
| CN106361455A (en) * | 2016-10-13 | 2017-02-01 | 成都优材科技有限公司 | 3D printing forming method for metal dental restoration |
| CN107470623A (en) * | 2017-08-30 | 2017-12-15 | 湖南顶立科技有限公司 | A kind of increasing material manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102006056045A1 (en) * | 2006-11-28 | 2008-06-05 | Hausch, Gernot, Dr. | Cobalt-based dental alloy for production of ceramic-veneered crowns, bridges and other restorations, contains nickel, chromium, molybdenum, tungsten and cobalt, optionally with small amounts of other elements |
| CN106361455A (en) * | 2016-10-13 | 2017-02-01 | 成都优材科技有限公司 | 3D printing forming method for metal dental restoration |
| CN107470623A (en) * | 2017-08-30 | 2017-12-15 | 湖南顶立科技有限公司 | A kind of increasing material manufacturing method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US11631600B2 (en) | 2017-08-24 | 2023-04-18 | Cerebras Systems Inc. | Apparatus and method for securing components of an integrated circuit |
| US11145530B2 (en) * | 2019-11-08 | 2021-10-12 | Cerebras Systems Inc. | System and method for alignment of an integrated circuit |
| CN113909497A (en) * | 2021-10-09 | 2022-01-11 | 江西金石三维智能制造科技有限公司 | Preparation method of selective laser melting cobalt-chromium alloy and cobalt-chromium denture alloy material |
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