CN117161388B - Low-oxygen-content titanium alloy powder and preparation method thereof - Google Patents

Low-oxygen-content titanium alloy powder and preparation method thereof Download PDF

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CN117161388B
CN117161388B CN202311457818.1A CN202311457818A CN117161388B CN 117161388 B CN117161388 B CN 117161388B CN 202311457818 A CN202311457818 A CN 202311457818A CN 117161388 B CN117161388 B CN 117161388B
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titanium alloy
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CN117161388A (en
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陈勇
刘宇
樊志钧
蔺庆山
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Tech Long Tianjin Metal Materials Co ltd
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Abstract

The application relates to the technical field of 3D printing, and particularly discloses low-oxygen-content titanium alloy powder and a preparation method thereof. The preparation method of the low-oxygen-content titanium alloy powder comprises the following steps: carrying out hydrogen absorption grinding treatment on the titanium alloy waste powder to obtain titanium hydride alloy powder, adding magnesium powder into the titanium hydride alloy powder, carrying out heat preservation reaction for 70-90h under the conditions that the temperature is 680-700 ℃ and the vacuum degree is 0.5-0.6Pa, and then carrying out spheroidization crushing to obtain titanium alloy powder with low oxygen content; wherein the weight ratio of the magnesium powder to the titanium hydride alloy powder is 1 (10-12). The oxygen content of the titanium alloy powder prepared by the preparation method is lower than 1300ppm, the requirement of the titanium alloy powder for 3D printing on the oxygen content is met, the titanium alloy powder can be continuously applied to the 3D printing technology, and the material cost of the titanium alloy powder for 3D printing is greatly reduced.

Description

Low-oxygen-content titanium alloy powder and preparation method thereof
Technical Field
The application relates to the technical field of 3D printing, in particular to a low-oxygen-content spheroidal titanium alloy powder and a preparation method thereof.
Background
3D printing, also called additive manufacturing, belongs to one of rapid prototyping technologies, and is based on digital model files, and an object is constructed by applying powdery metal or plastic and other bondable materials in a layer-by-layer printing mode. Titanium and titanium alloy are important metals developed in the middle of the twentieth century, and titanium alloy powder has the characteristics of low density, high strength, corrosion resistance, no magnetism and the like, and is a key raw material of 3D printing technology.
Currently, titanium alloy powder for 3D printing on the market is mostly manufactured by a rotating electrode method, wherein a titanium alloy electrode rod is used as a consumable electrode, electrons or ion current is received under a high-speed rotating state, the end of the consumable electrode is fused into liquid, the liquid is thrown out under the action of centrifugal force to form fine liquid drops, and the fine liquid drops are solidified into spherical titanium alloy powder particles under the action of surface tension. The titanium alloy powder prepared by the method has the advantages of high sphericity, high smoothness, no agglomeration phenomenon, good fluidity, high densification degree of printed products and the like, and the preparation method generally adopts inert gas for protection, does not need crucible smelting, effectively avoids the introduction of impurities, and has higher purity.
However, since the particle size range of the titanium alloy powder produced by the rotary electrode method is usually between 0 and 250 μm, only the titanium alloy powder having a particle size distribution of between 20 and 63 μm can be used in 3D printing, which makes the material cost of the titanium alloy powder for 3D printing always high. Therefore, in order to reduce the material cost of the titanium alloy powder for 3D printing, it is necessary to recycle the titanium alloy waste powder having a particle diameter of more than 63 μm. However, the recycling of the titanium alloy waste powder (for example, the secondary atomization of the titanium alloy waste powder at a high temperature by adopting a plasma method) by using the existing method generally increases the oxygen content of the titanium alloy waste powder by 300-500ppm, so that the oxygen content of the recycled titanium alloy powder reaches 1300-1800ppm, the oxygen content requirement of the titanium alloy powder for 3D printing (less than 1300 ppm) can not be met, and the titanium alloy waste powder can not be continuously applied to the 3D printing technology.
Disclosure of Invention
In order to solve the problems, the application provides titanium alloy powder with low oxygen content and a preparation method thereof.
In a first aspect, the present application provides a method for preparing a low oxygen content titanium alloy powder, which adopts the following technical scheme:
a method for preparing low oxygen content titanium alloy powder, comprising the following steps:
carrying out hydrogen absorption grinding treatment on the titanium alloy waste powder to obtain titanium hydride alloy powder, adding magnesium powder into the titanium hydride alloy powder, carrying out heat preservation reaction for 70-90h under the conditions that the temperature is 680-700 ℃ and the vacuum degree is 0.5-0.6Pa, and then carrying out crushing spheroidization to obtain low-oxygen-content titanium alloy powder; wherein the weight ratio of the magnesium powder to the titanium hydride alloy powder is 1 (10-12).
By adopting the technical scheme, the method utilizes the reversible characteristics of titanium and hydrogen, firstly prepares titanium alloy waste powder with the particle size larger than 63 mu m by hydrogen absorption treatment, then carries out dehydrogenation treatment on the titanium alloy powder, carries out oxygen reduction process by taking magnesium powder as a reducing agent while carrying out dehydrogenation treatment, and then carries out crushing and spheroidizing, so that the oxygen content of the recovered titanium alloy powder is lower than 1300ppm, the requirement of the titanium alloy powder for 3D printing on the oxygen content is met, the method can be continuously applied to 3D printing technology, and the material cost of the titanium alloy powder for 3D printing is greatly reduced.
Preferably, the magnesium powder is filled into the porous titanium tube and then added into the titanium hydride alloy powder.
Through adopting above-mentioned technical scheme, this application utilizes the magnesium powder steam that overflows in the hole of distributing on the porous titanium pipe to carry out oxygen reduction to dehydrogenated titanium powder for magnesium powder and titanium hydride alloy powder need not directly contact, show the difficult degree of follow-up separation magnesium powder, improved production efficiency, reduced manufacturing cost. In addition, as the chemical property of titanium is relatively active, the titanium is easy to react with other metals at high temperature, so that the titanium filter tube is used for loading magnesium powder, and the possibility of introducing impurities can be reduced.
Preferably, the air permeability of the porous titanium tube is 0.8-2L/cm 2 ·min·pa。
Through adopting above-mentioned technical scheme, the air permeability of porous titanium pipe has been optimized to this application for magnesium powder steam can fully contact with the titanium powder after the dehydrogenation, has improved the sufficiency of magnesium powder steam to titanium powder oxygen reduction process, thereby has reduced the oxygen content of the titanium alloy powder after retrieving.
Preferably, the pore diameter of the porous titanium tube is 0.1-10 mu m, and the particle diameter of the magnesium powder is 10-20 mu m.
By adopting the technical scheme, the pore diameter of the porous titanium tube and the particle size of the magnesium powder are limited, the possibility that the magnesium powder overflows from the pores on the surface of the porous titanium tube is reduced, and the purity of the recycled titanium alloy powder is improved.
Preferably, the hydrogen absorption treatment comprises a hydrogen absorption process and a grinding process, wherein the hydrogen absorption process specifically comprises the following steps: and (3) carrying out hydrogen absorption on the titanium alloy waste powder under the conditions that the temperature is 550-560 ℃ and the pressure is 0.03-0.05MPa, and stopping hydrogen absorption when the weight of the titanium alloy waste powder is increased by at least 3.2%.
Preferably, the particle size of the titanium alloy waste powder is 63-250 mu m.
Preferably, the grinding process specifically comprises the following steps: grinding and spheroidizing the waste titanium alloy powder after hydrogen absorption under the condition that the pressure of inert gas is maintained at 530-550KPa, and obtaining the hydrogenated titanium alloy powder with the particle size of 20-63 mu m under the condition that the rotating speed is 4500-5000 r/min.
By adopting the technical scheme, the titanium in the titanium alloy waste powder with the particle size of 63-250 mu m is fully and completely converted into titanium hydride through hydrogen absorption, and then the titanium is ground to 20-63 mu m, at the moment, the oxygen content in the titanium hydride alloy powder is less than 1800ppm, the nitrogen content is less than 200ppm, and the hydrogen content is less than 32000ppm.
Preferably, the crushing and spheroidizing specifically comprises: under the condition that the inert gas is maintained at 600-650MPa, the titanium alloy powder after dehydrogenation reduction is spheroidized and crushed under the condition that the rotating speed is 5500-6000 r/min.
By adopting the technical scheme, the titanium alloy powder subjected to dehydrogenation reduction is subjected to secondary spheroidization crushing to obtain the spheroidal titanium alloy powder, and the spheroidal titanium alloy powder can be directly used in 3D printing.
In a second aspect, the present application provides a low oxygen titanium alloy powder produced by the above-described production method.
Preferably, the oxygen content of the low oxygen content titanium alloy powder is less than 1300ppm.
Through adopting above-mentioned technical scheme, the low oxygen content titanium alloy powder that this application made has lower oxygen content, and its oxygen content is less than 1300ppm, satisfies 3D and prints with titanium alloy powder to the requirement of oxygen content, can directly be applied to 3D and print, has reduced 3D and has printed with titanium alloy powder's material cost.
In summary, the present application has the following beneficial technical effects:
1. the titanium alloy powder prepared by the preparation method has the oxygen content of less than 1300ppm, the nitrogen content of less than 200ppm and the hydrogen content of less than 200ppm, meets the requirement of the titanium alloy powder for 3D printing on the oxygen content, and can be directly applied to 3D printing;
2. the preparation method of the titanium alloy powder realizes the aim of recycling the titanium alloy waste powder with the particle size larger than 63 mu m, and greatly reduces the material cost of the titanium alloy powder for 3D printing;
3. the preparation method has the advantages of simple steps, easy operation, lower raw material cost and suitability for large-scale industrial production.
Detailed Description
The present application is described in further detail below in connection with examples, comparative examples and application examples.
The titanium alloy waste powder is titanium alloy spherical powder with the particle size of 63-250 mu m prepared by using a titanium alloy electrode rod as a consumable electrode through a rotary electrode method, and has the oxygen content of less than 700ppm, the nitrogen content of less than 100ppm and the hydrogen content of less than 100ppm;
the size of the porous titanium tube is phi 70mm multiplied by phi 50mm multiplied by 300mm, and the aperture is 0.1-10 mu m;
the purity of the magnesium powder is more than 99.9 percent, and the grain diameter is 10-20 mu m.
Examples 1.1.1 to 1.1.3
A method for preparing low oxygen content titanium alloy powder, comprising the following steps:
(1) Placing the titanium alloy waste powder with the particle size of 63-250 mu m into a hydrogen absorption furnace, absorbing hydrogen at the temperature of 550 ℃ and the pressure of 0.03-0.05MPa, and stopping absorbing hydrogen when the weight of the titanium alloy waste powder is increased by at least 3.2%;
(2) Putting the product obtained in the step (1) into an air flow mill, and grinding at a grinding chamber pressure of 530KPa and a grinding speed of 80kg/h under the protection of argon gas at a rotating speed of 4500r/min to obtain titanium hydride alloy powder with a particle size of 20-63 mu m;
(3) Filling magnesium powder into the material with air permeability of 0.5L/cm 2 In a porous titanium tube of min pa, and co-operating with the titanium hydride alloy powder obtained in step (2)Placing the mixture into a dehydrogenation furnace, carrying out heat preservation reaction for 70 hours under the conditions of 680 ℃ and 0.5Pa of vacuum degree, and then carrying out secondary spheroidizing crushing under the protection of argon gas at the speed of 5500r/min and the pressure of 600MPa, wherein the speed is 80kg/h, so as to obtain low-oxygen-content titanium alloy powder;
wherein examples 1.1.1-1.1.3 differ in that: the weight ratio of magnesium powder to titanium hydride alloy powder is different, specifically,
in example 1.1.1, the weight ratio of magnesium powder to titanium hydride alloy powder is 1:10, wherein the magnesium powder is 10kg, and the titanium hydride alloy powder is 100kg;
in example 1.1.2, the weight ratio of magnesium powder to titanium hydride alloy powder was 1:11, wherein the magnesium powder was 9.09kg and the titanium hydride alloy powder was 100kg;
in example 1.1.3, the weight ratio of magnesium powder to titanium hydride alloy powder was 1:12, wherein the magnesium powder was 8.33kg and the titanium hydride alloy powder was 100kg.
Examples 1.2.1 to 1.2.3
A method for preparing low oxygen content titanium alloy powder, comprising the following steps:
(1) Placing the titanium alloy waste powder with the particle size of 63-250 mu m into a hydrogen absorption furnace, absorbing hydrogen at the temperature of 555 ℃ and the pressure of 0.03-0.05MPa, and stopping absorbing hydrogen when the weight of the titanium alloy waste powder is increased by at least 3.2%;
(2) Putting the product obtained in the step (1) into an air flow mill, and grinding at a speed of 4700r/min and a grinding chamber pressure of 540KPa under the protection of argon gas, wherein the grinding speed is 100kg/h, so as to obtain titanium hydride alloy powder with a particle size of 20-63 mu m;
(3) Filling magnesium powder into the material with air permeability of 0.5L/cm 2 Placing the titanium alloy powder and the titanium alloy powder obtained in the step (2) into a dehydrogenation furnace together, carrying out heat preservation reaction for 80 hours under the conditions that the temperature is 690 ℃ and the vacuum degree is 0.55Pa, and then carrying out secondary spheroidization crushing under the protection of argon at the speed of 5700r/min and the pressure of 630MPa, wherein the speed is 100kg/h, so as to obtain the low-oxygen-content titanium alloy powder;
wherein examples 1.2.1-1.2.3 differ in that: the weight ratio of magnesium powder to titanium hydride alloy powder is different, specifically,
in example 1.2.1, the weight ratio of magnesium powder to titanium hydride alloy powder was 1:10, wherein the magnesium powder was 10kg and the titanium hydride alloy powder was 100kg;
in example 1.2.2, the weight ratio of magnesium powder to titanium hydride alloy powder was 1:11, wherein the magnesium powder was 9.09kg and the titanium hydride alloy powder was 100kg;
in example 1.2.3, the weight ratio of magnesium powder to titanium hydride alloy powder was 1:12, wherein the magnesium powder was 8.33kg and the titanium hydride alloy powder was 100kg.
Examples 1.3.1 to 1.3.3
A method for preparing low oxygen content titanium alloy powder, comprising the following steps:
(1) Placing the titanium alloy waste powder with the particle size of 63-250 mu m into a hydrogen absorption furnace, absorbing hydrogen at the temperature of 560 ℃ and the pressure of 0.03-0.05MPa, and stopping absorbing hydrogen when the weight of the titanium alloy waste powder is increased by at least 3.2%;
(2) Putting the product obtained in the step (1) into an air flow mill, and grinding at a speed of 5000r/min and a grinding chamber pressure of 550KPa under the protection of argon, wherein the grinding speed is 120kg/h, so as to obtain titanium hydride alloy powder with a particle size of 20-63 mu m;
(3) Filling magnesium powder into the material with air permeability of 0.5L/cm 2 Placing the titanium alloy powder and the titanium alloy powder obtained in the step (2) into a dehydrogenation furnace together in a porous titanium tube with the temperature of min Pa, and carrying out heat preservation reaction for 90 hours under the condition that the temperature is 700 ℃ and the vacuum degree is 0.6Pa to obtain titanium alloy powder with low oxygen content;
wherein examples 1.3.1-1.3.3 differ in that: the weight ratio of magnesium powder to titanium hydride alloy powder is different, specifically,
in example 1.3.1, the weight ratio of magnesium powder to titanium hydride alloy powder was 1:10, wherein the magnesium powder was 10kg and the titanium hydride alloy powder was 100kg;
in example 1.3.2, the weight ratio of magnesium powder to titanium hydride alloy powder was 1:11, wherein the magnesium powder was 9.09kg and the titanium hydride alloy powder was 100kg;
in example 1.3.3, the weight ratio of magnesium powder to titanium hydride alloy powder was 1:12, wherein the magnesium powder was 8.33kg and the titanium hydride alloy powder was 100kg.
Examples 2.1.1 to 2.1.3
A method for preparing low oxygen content titanium alloy powder, which is different from examples 1.1.1-1.1.3 in that: the air permeability of the porous titanium tube in the step (3) is 0.8-2L/cm 2 Min pa, wherein,
in example 2.1.1, the porous titanium tube had an air permeability of 0.8L/cm 2 ·min·pa;
In example 2.1.2, the porous titanium tube had an air permeability of 1.4L/cm 2 ·min·pa;
In example 2.1.3, the porous titanium tube had an air permeability of 2L/cm 2 ·min·pa。
Examples 2.2.1 to 2.2.3
A method for preparing low oxygen content titanium alloy powder, which is different from examples 1.2.1-1.2.3 in that: the air permeability of the porous titanium tube in the step (3) is 0.8-2L/cm 2 Min pa, wherein,
in example 2.2.1, the porous titanium tube had an air permeability of 0.8L/cm 2 ·min·pa;
Example 2.2.2 the porous titanium tube had an air permeability of 1.4L/cm 2 ·min·pa;
In example 2.2.3, the porous titanium tube had an air permeability of 2L/cm 2 ·min·pa。
Examples 2.3.1 to 2.3.3
A method for preparing low oxygen content titanium alloy powder, which is different from examples 1.3.1-1.3.3 in that: the air permeability of the porous titanium tube in the step (3) is 0.8-2L/cm 2 Min pa, wherein,
in example 2.3.1, the porous titanium tube had an air permeability of 0.8L/cm 2 ·min·pa;
In example 2.3.2, the porous titanium tube had an air permeability of 1.4L/cm 2 ·min·pa;
In example 2.3.3, the porous titanium tube had an air permeability of 2L/cm 2 ·min·pa。
Comparative examples 1.1.1 to 1.1.3
The differences from examples 1.1.1 to 1.1.3 are: in the step (3), the porous titanium tube filled with magnesium powder is not added into the dehydrogenation furnace, and only the titanium hydride alloy powder obtained in the step (2) is put into the dehydrogenation furnace, and the rest steps are the same as those of the examples 1.1.1-1.1.3.
Comparative examples 1.2.1 to 1.2.3
The differences from examples 1.2.1-1.2.3 are: in the step (3), the porous titanium tube filled with magnesium powder is not added into the dehydrogenation furnace, and only the titanium hydride alloy powder obtained in the step (2) is put into the dehydrogenation furnace, and the rest steps are the same as those of the examples 1.2.1-1.2.3.
Comparative examples 1.3.1 to 1.3.3
The differences from examples 1.3.1-1.3.3 are: in the step (3), the porous titanium tube filled with magnesium powder is not added into the dehydrogenation furnace, and only the titanium hydride alloy powder obtained in the step (2) is put into the dehydrogenation furnace, and the rest steps are the same as those of the examples 1.3.1-1.3.3.
Comparative examples 2.1.1 to 2.1.3
The differences from examples 1.1.1 to 1.1.3 are: in the step (3), aluminum powder is used for replacing magnesium powder by equal amount to be filled into the porous titanium tube, and the rest steps are the same as those of the embodiment 1.1.1-1.1.3.
Comparative examples 2.2.1 to 2.2.3
The differences from examples 1.2.1-1.2.3 are: in the step (3), aluminum powder is used for replacing magnesium powder by equal amount to be filled into the porous titanium tube, and the rest steps are the same as those of the embodiment 1.2.1-1.2.3.
Comparative examples 2.3.1 to 2.3.3
The differences from examples 1.3.1-1.3.3 are: in the step (3), aluminum powder is used for replacing magnesium powder by equal amount to be filled into the porous titanium tube, and the rest steps are the same as those of the embodiment 1.3.1-1.3.3.
Comparative examples 3.1.1 to 3.1.3
The differences from examples 1.1.1 to 1.1.3 are: in the step (3), the weight ratio of magnesium powder to titanium hydride alloy powder is 1:20, and the rest steps are the same as those of the embodiment 1.1.1-1.1.3; wherein,
in comparative example 3.1.1, 5kg of magnesium powder and 100kg of titanium hydride alloy powder;
in comparative example 3.1.2, 5kg of magnesium powder and 100kg of titanium hydride alloy powder;
in comparative example 3.1.3, 5kg of magnesium powder and 100kg of titanium hydride alloy powder were used.
Comparative examples 3.2.1 to 3.2.3
The differences from examples 1.2.1-1.2.3 are: in the step (3), the weight ratio of magnesium powder to titanium hydride alloy powder is 1:15, and the rest steps are the same as those of the embodiment 1.2.1-1.2.3; wherein,
comparative example 3.2.1, magnesium powder was 6.67kg and titanium hydride alloy powder was 100kg;
comparative example 3.2.2, magnesium powder 6.67kg, titanium hydride alloy powder 100kg;
in comparative example 3.2.3, 6.67kg of magnesium powder and 100kg of titanium hydride alloy powder were used.
Comparative examples 3.3.1 to 3.3.3
The differences from examples 1.3.1-1.3.3 are: in the step (3), the weight ratio of magnesium powder to titanium hydride alloy powder is 1:18, and the rest steps are the same as those of the embodiment 1.3.1-1.3.3; wherein,
comparative example 3.3.1, 5.56kg of magnesium powder and 100kg of titanium hydride alloy powder;
comparative example 3.3.2, 5.56kg of magnesium powder and 100kg of titanium hydride alloy powder;
in comparative example 3.3.3, 5.56kg of magnesium powder and 100kg of titanium hydride alloy powder were used.
Comparative examples 4.1.1 to 4.1.3
The differences from examples 1.1.1 to 1.1.3 are: in the step (3), the reaction time was 60 hours, and the rest of the steps were the same as in examples 1.1.1 to 1.1.3.
Comparative examples 4.2.1 to 4.2.3
The differences from examples 1.2.1-1.2.3 are: in the step (3), the reaction time was 90.5 hours, and the rest of the steps were the same as in examples 1.2.1 to 1.2.3.
Comparative examples 4.3.1 to 4.3.3
The differences from examples 1.3.1-1.3.3 are: in the step (3), the reaction time was 91 hours, and the rest of the steps were the same as in examples 1.3.1 to 1.3.3.
Performance detection
The low oxygen content titanium alloy powders prepared in examples 1-2 and comparative examples 1-4 were subjected to elemental analysis using an oxygen-nitrogen-hydrogen analyzer, respectively, and their corresponding oxygen content, nitrogen content and hydrogen content were recorded in table 1.
Table 1 table of performance test data
Project Oxygen content (ppm) Nitrogen content (ppm) Hydrogen content (ppm)
Example 1.1.1 935 185 171
Example 1.1.2 928 183 168
Example 1.1.3 921 180 165
Example 1.2.1 933 179 165
Example 1.2.2 925 178 163
Example 1.2.3 919 175 160
Example 1.3.1 934 182 168
Example 1.3.2 926 180 166
Example 1.3.3 919 178 164
Example 2.1.1 925 181 170
Example 2.1.2 917 180 166
Example 2.1.3 911 176 163
Example 2.2.1 921 175 164
Example 2.2.2 915 174 162
Example 2.2.3 908 171 158
Example 2.3.1 923 177 166
Example 2.3.2 917 175 164
Example 2.3.3 910 174 161
Comparative example 1.1.1 2730 185 170
Comparative example 1.1.2 2725 182 168
Comparative example 1.1.3 2718 180 166
Comparative example 1.2.1 2727 178 165
Comparative example 1.2.2 2721 178 163
Comparative example 1.2.3 2715 176 160
Comparative example 1.3.1 2728 182 169
Comparative example 1.3.2 2723 180 165
Comparative example 1.3.3 2715 178 163
Comparative example 2.1.1 1352 185 170
Comparative example 2.1.2 1347 183 168
Comparative example 2.1.3 1340 180 166
Comparative example 2.2.1 1349 179 165
Comparative example 2.2.2 1344 178 162
Comparative example 2.2.3 1337 175 160
Comparative example 2.3.1 1351 182 169
Comparative example 2.3.2 1345 180 166
Comparative example 2.3.3 1339 178 164
Comparative example 3.1.1 1229 186 171
Comparative example 3.1.2 1224 182 168
Comparative example 3.1.3 1220 180 165
Comparative example 3.2.1 1226 179 165
Comparative example 3.2.2 1221 178 163
Comparative example 3.2.3 1218 174 160
Comparative example 3.3.1 1228 182 168
Comparative example 3.3.2 1222 180 166
Comparative example 3.3.3 1219 178 164
Comparative example 4.1.1 1209 205 337
Comparative example 4.1.2 1204 203 334
Comparative example 4.1.3 1198 200 330
Comparative example 4.2.1 931 179 164
Comparative example 4.2.2 924 178 163
Comparative example 4.2.3 918 175 160
Comparative example 4.3.1 931 182 164
Comparative example 4.3.2 925 180 163
Comparative example 4.3.3 918 178 160
As can be seen from Table 1, the recovered titanium alloy powder prepared in the embodiment of the application has the oxygen content of less than 1300ppm, the nitrogen content of less than 200ppm and the hydrogen content of less than 200ppm, and experimental data show that the method for recovering the titanium alloy waste powder with the particle size of 63-250 mu m does not increase the oxygen content of the titanium alloy waste powder, and the recovered titanium alloy powder still has lower oxygen content and meets the requirement of the titanium alloy powder for 3D printing on the oxygen content.
As can be seen from the data of each group of the examples 2 and 1, the porous titanium tube has further controlled air permeability, so that more magnesium powder steam can overflow from the porous titanium tube, the sufficiency of the magnesium powder steam for the oxygen reduction process of the titanium powder is improved, and the oxygen content of the recovered titanium alloy powder is further reduced.
Comparative example 1 is different from example 1 in that only the titanium hydride alloy powder was subjected to the dehydrogenation treatment without using magnesium powder for the oxygen reduction process, and as can be seen from table 1, the recovered titanium alloy powder obtained in comparative example 1 has an oxygen content of 2715 to 2730ppm, which is significantly higher than that of example 1, and experimental data shows that the oxygen content in the titanium alloy powder can be significantly reduced by using magnesium powder for the oxygen reduction process while the dehydrogenation process is performed.
Comparative example 2 is different from example 1 in that the titanium alloy powder was subjected to the oxygen reduction process using aluminum powder instead of magnesium powder, and as can be seen from table 1, the recovered titanium alloy powder obtained in comparative example 2 has an oxygen content of 1337-1352ppm, which is significantly higher than that of example 1, and experimental data shows that the magnesium powder has a more remarkable oxygen reduction effect on the titanium alloy powder, and the oxygen content in the obtained titanium alloy powder is lower.
Comparative example 3 is different from example 1 in that the weight ratio of magnesium powder to titanium hydride alloy powder is not within the scope of the present application, and as can be seen from table 1, the oxygen content of the recovered titanium alloy powder obtained in comparative example 3 is 1218-1229ppm, which is significantly higher than that of example 1, and experimental data shows that the oxygen content of the recovered titanium alloy powder can be reduced by controlling the weight ratio of magnesium powder to titanium hydride alloy powder.
Comparative example 4 differs from example 1 in that the incubation time in step (3) is different, wherein comparative example 4.1 differs from example 1.1 in that the incubation time is shortened, and as can be seen from table 1, the oxygen content of the recovered titanium alloy powder obtained in comparative example 4.1 is 1198-1209ppm, which is significantly higher than that in example 1.1, and experimental data shows that too short incubation time affects the sufficient progress of the oxygen reduction of magnesium powder, thereby making the oxygen content in the recovered titanium alloy powder higher; comparative examples 4.2 to 4.3 are different from examples 1.2 to 1.3 in that the incubation time is slightly prolonged, and as can be seen from table 1, the oxygen content of the recovered titanium alloy powder obtained in comparative examples 4.2 to 4.3 is 918 to 931ppm, which is almost the same as that in examples 1.2 to 1.3, and experimental data indicate that the incubation time is prolonged again on the basis of the present application, and the oxygen content in the titanium alloy powder cannot be reduced continuously, but the production energy consumption is increased, and the production cost is increased.
The embodiments of the present invention are all preferred embodiments of the present application, and are not intended to limit the scope of the present application in this way, therefore: all equivalent changes in structure, shape and principle of this application should be covered in the protection scope of this application.

Claims (8)

1. A method for preparing low-oxygen-content titanium alloy powder, which is characterized by comprising the following steps:
carrying out hydrogen absorption grinding treatment on the titanium alloy waste powder to obtain titanium hydride alloy powder, adding magnesium powder into the titanium hydride alloy powder, carrying out heat preservation reaction for 70-90h under the conditions that the temperature is 680-700 ℃ and the vacuum degree is 0.5-0.6Pa, and then carrying out crushing spheroidization to obtain low-oxygen-content titanium alloy powder; wherein, the weight ratio of the magnesium powder to the titanium hydride alloy powder is 1 (10-12);
firstly filling the magnesium powder into a porous titanium tube, and then adding the magnesium powder into titanium hydride alloy powder;
the air permeability of the porous titanium tube is 0.8-2L/cm 2 ·min·pa。
2. The method for preparing the low-oxygen-content titanium alloy powder according to claim 1, wherein: the pore diameter of the porous titanium tube is 0.1-10 mu m, and the particle diameter of the magnesium powder is 10-20 mu m.
3. The method for preparing low-oxygen-content titanium alloy powder according to claim 1, wherein the hydrogen-absorbing grinding treatment comprises a hydrogen-absorbing process and a grinding process, wherein the hydrogen-absorbing process is specifically as follows: and (3) carrying out hydrogen absorption on the titanium alloy waste powder under the conditions that the temperature is 550-560 ℃ and the pressure is 0.03-0.05MPa, and stopping hydrogen absorption when the weight of the titanium alloy waste powder is increased by at least 3.2%.
4. A method for preparing a low oxygen content titanium alloy powder according to claim 3, wherein: the particle size of the titanium alloy waste powder is 63-250 mu m.
5. A method for preparing a low oxygen content titanium alloy powder according to claim 3, wherein the grinding process is specifically: grinding and spheroidizing the waste titanium alloy powder after hydrogen absorption under the condition that the pressure of inert gas is maintained at 530-550KPa, and obtaining the hydrogenated titanium alloy powder with the particle size of 20-63 mu m under the condition that the rotating speed is 4500-5000 r/min.
6. The method for preparing low-oxygen-content titanium alloy powder according to claim 1, wherein the crushing and spheroidizing is specifically: under the condition that the inert gas is maintained at 600-650MPa, the titanium alloy powder after dehydrogenation reduction is spheroidized and crushed under the condition that the rotating speed is 5500-6000 r/min.
7. A low oxygen content titanium alloy powder produced by the production method of the low oxygen content titanium alloy powder as claimed in any one of claims 1 to 6.
8. The low oxygen titanium alloy powder of claim 7, wherein: the oxygen content of the low oxygen content titanium alloy powder is less than 1300ppm.
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