Method for protecting titanium alloy samples during heat treatment

Abstract

The application belongs to the technical field of non-ferrous metal processing and relates to a protection method for a titanium alloy sample during heat treatment. The titanium alloy sample is first placed at the bottom of a preset hole of a titanium alloy base. Then, a sealing sample block, fine-grained titanium sponge and large-grained titanium sponge are sequentially placed until the preset hole of the titanium alloy base is filled. Finally, plasma welding box packaging is performed, so that the titanium alloy sample is packaged in the titanium alloy base, thereby solving the pollution and oxidation problems of the titanium alloy sample during heat treatment in the process of titanium alloy research.

Description

Technical Field

[0001] This invention belongs to the field of non-ferrous metal processing technology and relates to a method for protecting titanium alloy samples during heat treatment. Background Technology

[0002] It is well known in the industry that titanium alloys possess excellent specific strength, specific stiffness, and corrosion resistance, making them widely used in aerospace and biomedical fields. Due to the diverse performance requirements of titanium alloys across different applications, heat treatment is often used to adjust the microstructure and phase content of the alloy to meet these requirements. Therefore, research on the microstructure evolution during the heat treatment process of titanium alloys is crucial.

[0003] Because titanium is extremely reactive at high temperatures, studies comparing the microstructure of titanium alloys before and after heat treatment often lead to controversial results due to factors such as sample oxidation and contamination. Currently, common protection methods for high-temperature heat-treated titanium alloys include vacuum equipment or inert gas protection equipment. However, these methods have relatively high equipment requirements, resulting in high experimental costs. Therefore, practical sample protection methods are still lacking in engineering applications.

[0004] In view of this, the present invention is hereby proposed. Summary of the Invention

[0005] The purpose of this invention is to overcome the shortcomings of the prior art and provide a method for protecting titanium alloy samples during heat treatment. By encapsulating the titanium alloy sample, the surface of the sample remains intact after high-temperature heat treatment in atmospheric conditions.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] This method of protecting titanium alloy samples during heat treatment involves first placing the titanium alloy sample at the bottom of a pre-placed hole in the titanium alloy substrate; then sequentially placing a sealing sample block, fine-particle sponge titanium, and large-particle sponge titanium until the pre-placed hole in the titanium alloy substrate is filled; finally, plasma welding is performed to encapsulate the titanium alloy sample within the titanium alloy substrate.

[0008] Furthermore, the specific steps of the above-mentioned method for protecting titanium alloy samples during heat treatment are as follows:

[0009] Step 1: Based on the size of the titanium alloy sample to be heat-treated, prepare a titanium alloy substrate of the corresponding size, and open a pre-set hole for placing the titanium alloy sample on the titanium alloy substrate. Measure and record the depth and specific location information of the pre-set hole.

[0010] Step 2: Place the titanium alloy sample to be treated into the bottom of the pre-set hole;

[0011] Step 3: Place a sealing sample block in the pre-set hole above the titanium alloy sample, and then fill it with fine-particle sponge titanium and large-particle sponge titanium in sequence until the pre-set hole of the titanium alloy matrix is ​​filled.

[0012] Step 4: Place the titanium alloy substrate treated in Step 3 into a vacuum plasma welding box and weld the sponge titanium filling the holes to completely weld the upper layer of the holes.

[0013] Step 5: Heat treat the titanium alloy substrate after step 4, and then cut the titanium alloy sample according to the depth and specific location information of the pre-set hole in step 1 to protect the titanium alloy sample during the heat treatment process.

[0014] Furthermore, the diameter of the circumcircle of the surface to be analyzed of the titanium alloy sample in step 1 is ≤50mm.

[0015] Furthermore, in step 1, the titanium alloy substrate is a titanium alloy block material, the diameter of the inscribed circle of the punched surface of the titanium alloy block material is ≥42mm, the length of the titanium alloy block material is ≥80mm, and the depth of the pre-drilled hole in the titanium alloy block material is ≥40mm.

[0016] Furthermore, the titanium alloy block material is an ingot riser, a forged billet head, or other blocky titanium alloy scrap.

[0017] Furthermore, the diameter of the pre-placed hole in the titanium alloy block material is 2 mm larger than the diameter of the circumcircle of the surface to be analyzed of the titanium alloy sample.

[0018] Furthermore, in step 2, the surface of the titanium alloy sample to be analyzed faces the bottom of the pre-set hole.

[0019] Furthermore, the particle size of the fine-particle sponge titanium in step 3 is 0-5.0 mm, and the particle size of the large-particle sponge titanium is 5.0-12.0 mm.

[0020] Furthermore, the welding process parameters in step 4 are as follows: pre-vacuum ≤10Pa, leakage rate ≤5Pa / min, welding current: 100~600A, welding voltage: 30~100V, welding time ≥3min, and post-weld cooling time ≥10min.

[0021] Furthermore, the process parameters for heat treatment in step 5 are as follows: heat treatment temperature ≤1250℃, total heat treatment time ≤250h.

[0022] Compared with the prior art, the technical solution provided by the present invention has the following beneficial effects: The present invention protects the titanium alloy sample in the pre-placed hole of the titanium alloy substrate by placing the titanium alloy sample into the pre-placed hole of the titanium alloy substrate, sealing it with a sealing sample block and sponge titanium in sequence, and then welding it with a plasma welding box. Finally, heat treatment is performed to solve the pollution and oxidation problems caused by heat treatment of titanium alloy samples in the process of titanium alloy research. Attached Figure Description

[0023] The accompanying drawings are incorporated in and form part of this specification, and together with the description serve to explain the principles of the invention.

[0024] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, for those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0025] Figure 1 A flowchart of a method for protecting titanium alloy samples during heat treatment provided by the present invention;

[0026] Figure 2 This is a structural layout diagram of the titanium alloy sample during heat treatment and protection, as provided by the present invention.

[0027] The components are: 1. Titanium alloy sample; 2. Titanium alloy matrix; 3. Pre-placed hole; 4. Sealed sample block; 5. Fine-grained sponge titanium; 6. Large-grained sponge titanium; 7. Surface to be analyzed. Detailed Implementation

[0028] Exemplary embodiments will now be described in detail, examples of which are illustrated in the accompanying drawings. When the following description relates to the drawings, unless otherwise indicated, the same numbers in different drawings denote the same or similar elements. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples consistent with some aspects of the invention as detailed in the appended claims.

[0029] This invention provides a method for protecting titanium alloy samples during heat treatment, combined with... Figure 2 As shown, the titanium alloy sample 1 is first placed at the bottom of the pre-set hole 3 of the titanium alloy substrate 2; then the sealing sample block 4, fine-particle sponge titanium 5, and large-particle sponge titanium 6 are placed in sequence until the pre-set hole 3 of the titanium alloy substrate 2 is filled; finally, plasma welding is performed to encapsulate the titanium alloy sample 1 in the titanium alloy substrate 2.

[0030] Furthermore, for the above protection methods, see [link to relevant documentation]. Figure 1 As shown, the specific steps are as follows:

[0031] Step 1: Based on the size of the titanium alloy sample 1 to be heat-treated, prepare a titanium alloy substrate 2 of the corresponding size, and open a pre-set hole 3 on the titanium alloy substrate 2 for placing the titanium alloy sample 1. Measure and record the depth and specific location information of the pre-set hole 3.

[0032] Step 2: Place the titanium alloy sample 1 to be processed into the bottom of the pre-set hole 3;

[0033] Step 3: Place a sealing sample block 4 in the pre-set hole 3 above the titanium alloy sample 1, and then fill in fine-particle sponge titanium 5 and large-particle sponge titanium 6 in sequence until the pre-set hole 3 of the titanium alloy substrate 2 is filled.

[0034] Step 4: Place the titanium alloy substrate 2 processed in Step 3 into a vacuum plasma welding box and weld the sponge titanium filling the holes to completely weld the upper layer of the holes.

[0035] Step 5: Heat treat the titanium alloy substrate 2 after step 4, and then cut the titanium alloy sample 1 according to the depth and specific location information of the pre-set hole 3 in step 1 to protect the titanium alloy sample 1 during the heat treatment process.

[0036] To enable those skilled in the art to better understand the technical solutions of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments.

[0037] Example 1

[0038] This embodiment provides a method for protecting titanium alloy samples during heat treatment, and the specific steps are as follows:

[0039] Step 1: Prepare the titanium alloy sample 1 to be heat-treated. Its overall shape is cylindrical, and the surface to be analyzed 7 is circular with a diameter of 8 mm and a cylinder height of 20 mm. According to the size of the titanium alloy sample 1 to be treated, select an ingot riser to encapsulate the titanium alloy sample 1. The diameter of the inscribed circle of the drilling surface of the ingot riser is 50 mm, and the length of the riser is 100 mm. Then, drill a hole at the center of the inscribed circle of the drilling surface of the riser to obtain the pre-set hole 3. The diameter of the pre-set hole 3 is 10 mm, and the depth of the pre-set hole 3 is 60 mm.

[0040] Step 2: Place the titanium alloy sample 1 to be heat-treated into the bottom of the pre-set hole 3;

[0041] Step 3: Place a cylindrical titanium alloy block with a diameter of 9mm and a height of 20mm into the pre-set hole 3, and then place fine-particle sponge titanium 5 (0-5mm) and large-particle sponge titanium 6 (5.0-10.0mm) into the pre-set hole 3 in sequence until the pre-set hole 3 is filled.

[0042] Step 4: Place the material (ingot riser) prepared in Step 3 into the vacuum plasma welding box. Before welding, measure the vacuum index. The pre-vacuum is 9.5 Pa and the leakage rate is 4.8 Pa / min. Then weld the pre-set hole 3. The welding current is 110 A, the welding voltage is 32 V, the welding time is 3 min, and then cool for 10 min before removing from the furnace.

[0043] Step 5: Place the ingot riser processed in Step 4 into a heat treatment furnace for heat treatment at a temperature of 650℃ for 12 hours. After heat treatment, cut the material according to the center of the inscribed circle and a depth of 60mm. After taking out the heat-treated sample, no oxidation phenomenon was found on the surface.

[0044] Example 2

[0045] This embodiment provides another method for protecting titanium alloy samples during heat treatment, and the specific steps are as follows:

[0046] Step 1: Prepare the titanium alloy sample 1 to be heat-treated. Its overall shape is a cuboid, and the surface to be analyzed 7 is rectangular. The diameter of the circumscribed circle of the surface to be analyzed 7 is 25 mm, and the length perpendicular to the direction of the surface to be analyzed 7 is 40 mm. According to the size of the titanium alloy sample 1 to be treated, select a titanium alloy scrap head to encapsulate the titanium alloy sample 1. The diameter of the inscribed circle of the drilled surface of the scrap head is 80 mm, and the length of the riser is 180 mm. Then, drill a hole at the center of the inscribed circle of the riser drilling surface to obtain the pre-set hole 3. The diameter of the pre-set hole 3 is 30 mm, and the depth of the pre-set hole 3 is 140 mm.

[0047] Step 2: Place the titanium alloy sample 1 to be heat-treated into the bottom of the pre-set hole 3;

[0048] Step 3: Place a cylindrical titanium alloy block with a diameter of 29mm and a height of 40mm into the pre-set hole 3, and then place fine-particle sponge titanium 5 (0-5mm) and large-particle sponge titanium 6 (5.0-12.0mm) into the pre-set hole 3 in sequence until the pre-set hole 3 is filled.

[0049] Step 4: Place the material (titanium alloy scrap) prepared in Step 3 into the vacuum plasma welding box. Before welding, measure the vacuum index. The pre-vacuum is 5.0 Pa and the leakage rate is 2.3 Pa / min. Then weld the pre-set hole 3. The welding current is 220 A, the welding voltage is 65 V, the welding time is 10 min, and then cool for 20 min before removing from the furnace.

[0050] Step 5: Place the titanium alloy scrap material processed in Step 4 into a heat treatment furnace for heat treatment at a temperature of 980℃ for 60 hours. After heat treatment, cut the material according to the center of the inscribed circle and a depth of 140mm. After taking out the heat-treated sample, no oxidation phenomenon was observed on the surface.

[0051] Example 3

[0052] This embodiment provides another method for protecting titanium alloy samples during heat treatment, and the specific steps are as follows:

[0053] Step 1: Prepare the titanium alloy sample 1 to be heat-treated. The sample is irregularly shaped, and the surface to be analyzed 7 is an irregular polygon with a diameter of 48 mm and a length of 100 mm perpendicular to the surface to be analyzed 7. Based on the dimensions of the titanium alloy sample 1, select a titanium alloy riser for sample encapsulation. The diameter of the inscribed circle of the riser drilling surface is 150 mm, and the riser length is 230 mm. Then, drill a hole at the center of the inscribed circle of the riser drilling surface to obtain a pre-drilled hole 3 with a diameter of 55 mm and a depth of 180 mm.

[0054] Step 2: Place the titanium alloy sample 1 to be heat-treated into the bottom of the pre-set hole 3;

[0055] Step 3: Place a cylindrical titanium alloy block with a diameter of 54mm and a height of 30mm into the pre-drilled hole 3, and then place fine-particle sponge titanium 5 (0-5mm) and large-particle sponge titanium 6 (5.0-12.0mm) in sequence until the drill hole is filled.

[0056] Step 4: Place the material (titanium alloy riser) prepared in Step 3 into the vacuum plasma welding box. Before welding, measure the vacuum index. The pre-vacuum is 2.0 Pa and the leakage rate is 0.8 Pa / min. Then weld the pre-set hole 3. The welding current is 580 A, the welding voltage is 95 V, the welding time is 15 min, and then cool for 40 min before removing it from the furnace.

[0057] Step 5: Place the titanium alloy riser prepared in Step 4 into a heat treatment furnace for heat treatment at a temperature of 1250℃ for 250 hours. After heat treatment, cut the material according to the center of the inscribed circle and a depth of 180mm. After taking out the heat-treated sample, no oxidation phenomenon was observed on the surface.

[0058] In summary, the method for protecting titanium alloy sample 1 during heat treatment provided by this invention can effectively solve the problems of contamination and oxidation of titanium alloy sample 1 during heat treatment, and reduce experimental costs.

[0059] The above description is merely a specific embodiment of the present invention, enabling those skilled in the art to understand or implement the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention.

[0060] It should be understood that the present invention is not limited to the content already described above, and various modifications and changes can be made without departing from its scope. The scope of the present invention is limited only by the appended claims.

Claims

1. A method for protecting titanium alloy samples during heat treatment, characterized in that, First, place the titanium alloy sample (1) into the bottom of the pre-placed hole (3) of the titanium alloy substrate (2); then place the sealed sample block (4), fine-particle sponge titanium (5), and large-particle sponge titanium (6) in sequence until the pre-placed hole (3) of the titanium alloy substrate (2) is filled; finally, perform plasma welding box encapsulation so that the titanium alloy sample (1) is encapsulated in the titanium alloy substrate (2). The specific steps are as follows: Step 1: Based on the size of the titanium alloy sample (1) to be heat-treated, prepare a titanium alloy substrate (2) of the corresponding size, and open a pre-set hole (3) on the titanium alloy substrate (2) for placing the titanium alloy sample (1), measure and record the depth and specific location information of the pre-set hole (3). Step 2: Place the titanium alloy sample (1) to be treated into the bottom of the pre-set hole (3); Step 3: Place a sealing sample block (4) in the pre-set hole (3) above the titanium alloy sample (1), and then fill in fine-particle sponge titanium (5) and large-particle sponge titanium (6) in sequence until the pre-set hole (3) of the titanium alloy substrate (2) is filled. Step 4: Place the titanium alloy substrate (2) after step 3 in a vacuum plasma welding box and weld the sponge titanium filling the holes so that the upper layer of the holes is completely welded. Step 5: Heat treat the titanium alloy substrate (2) after step 4 to protect the titanium alloy sample (1) during the heat treatment process. Then, cut the titanium alloy sample (1) according to the depth and specific location information of the pre-set hole (3) in step 1.

2. The method for protecting titanium alloy samples during heat treatment according to claim 1, characterized in that, The diameter of the circumscribed circle of the surface (7) to be analyzed in the titanium alloy sample (1) described in step 1 is ≤50mm.

3. The method for protecting titanium alloy samples during heat treatment according to claim 1, characterized in that, In step 1, the titanium alloy substrate (2) is a titanium alloy block material. The diameter of the inscribed circle of the punched surface of the titanium alloy block material is ≥42mm, the length of the titanium alloy block material is ≥80mm, and the depth of the pre-placed hole (3) of the titanium alloy block material is ≥40mm.

4. The method for protecting titanium alloy samples during heat treatment according to claim 3, characterized in that, The titanium alloy block material is an ingot riser, forging billet head, or other blocky titanium alloy scrap.

5. The method for protecting titanium alloy samples during heat treatment according to claim 3, characterized in that, The diameter of the pre-placed hole (3) of the titanium alloy block material is 2 mm larger than the diameter of the circumcircle of the surface (7) to be analyzed of the titanium alloy sample (1).

6. The method for protecting titanium alloy specimens during heat treatment according to claim 1, characterized in that, In step 2, the surface (7) of the titanium alloy sample (1) to be analyzed faces the bottom of the pre-set hole (3).

7. The method for protecting titanium alloy samples during heat treatment according to claim 1, characterized in that, The fine-particle sponge titanium (5) in step 3 has a particle size of less than or equal to 5.0 mm, and the large-particle sponge titanium (6) has a particle size of greater than 5.0 mm and less than or equal to 12.0 mm.

8. The method for protecting titanium alloy specimens during heat treatment according to claim 1, characterized in that, The welding process parameters in step 4 are as follows: pre-vacuum ≤10Pa, leakage rate ≤5Pa / min, welding current: 100~600A, welding voltage: 30~100V, welding time ≥3min, and post-weld cooling time ≥10min.

9. The method for protecting titanium alloy specimens during heat treatment according to claim 1, characterized in that, The process parameters for heat treatment in step 5 are as follows: heat treatment temperature ≤ 1250℃, total heat treatment time ≤ 250h.

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