KR101275054B1 - Method of manufacturing titanium alloy powder with low oxygen concentration - Google Patents

Abstract

PURPOSE: A manufacturing method of low-oxygen titanium alloy powder is provided to manufacture low-oxygen titanium alloy powder with the oxygen content below 2000 weight ppm by performing deoxidation for 1-3 hours at 950-1050 degrees centigrade by using 80-120 wt% of deoxidizer for 100 wt % of titanium alloy base powder. CONSTITUTION: A manufacturing method of low oxygen titanium alloy powder includes the following steps: a step of placing 80-120 wt% of deoxidizer in a lower container with an open top and placing 100 wt% of titanium allow base powder containing oxygen over 3000 weight ppm on a sieve of an upper container combined with the lower container and having a bottom surface made of the sieve(S110); a step of heating the inside of the lower container and upper container at 950-1050 degrees centigrade and deoxidizing the titanium alloy base powder for 1-3 hours in a vacuum of 1x10^(-5) torr by using the evaporation of the deoxidizer(S210); a step of washing and drying the deoxidized titanium alloy powder(S130). The titanium alloy base powder is Ti-6Al-4V, and the oxygen content of the titanium alloy powder obtained from the above step is 1760-2000 weight ppm. [Reference numerals] (AA) Start; (BB) End; (S110) Titanium alloy powder/deoxidizer; (S120) Deoxidation; (S130) Deoxidized titanium alloy powder

Description

Method for producing low oxygen titanium alloy powder {METHOD OF MANUFACTURING TITANIUM ALLOY POWDER WITH LOW OXYGEN CONCENTRATION}

The present invention relates to a method for producing a titanium alloy powder such as Ti-6Al-4V, and more particularly, to a method for producing a low oxygen titanium alloy powder having an oxygen content of 2,000 ppm or less.

Although titanium (Ti) alloy is a lightweight material, due to its high tensile strength and corrosion resistance, it is used in various fields such as aircraft, spacecraft, medical equipment, and sports equipment.

Commercial titanium alloy powders such as Ti-6Al-4V (% by weight, Ti: 90%, Al: 6%, V: 4%) contain approximately thousands of ppm by weight of oxygen. Due to such a high content of oxygen, in the case of a material made from titanium alloy powder, the desired physical properties are difficult to appear properly.

Therefore, it is necessary to lower the high oxygen content of such titanium alloy powder to produce titanium alloy powder of higher purity.

Background art related to the present invention is a method for producing a high purity titanium alloy powder disclosed in Korean Patent Publication No. 10-1014350 (2011.02.15.).

For the high purity titanium alloy powder production method described in the above document, it is carried out by titanium alloy surface reduction, washing, hydrogenation, grinding and dehydrogenation processes. However, in such a method, the oxygen content of the produced titanium alloy powder is about 2000 ppm by weight or more, and it is known that the oxygen content is still high.

Therefore, a technique for producing low oxygen titanium alloy powder having an oxygen content of 2000 ppm or less is required.

An object of the present invention is to provide a method for producing a low oxygen titanium alloy powder having a low oxygen content can exhibit a high deoxidation efficiency.

Method for producing a low oxygen titanium alloy powder according to an embodiment of the present invention for achieving the above object is (a) placing 80 to 120 parts by weight of the deoxidizer in the lower container is opened, the lower surface is coupled to the lower container Disposing 100 parts by weight of the titanium alloy powder on the sheave of the upper container which is made of the sieve; (b) heating the lower vessel and the upper vessel to 950-1050 ° C. to deoxidize the titanium alloy mother powder using the deoxidizer evaporation for 1-3 hours under vacuum; And (c) washing the deoxidized titanium alloy powder and drying the powder.

At this time, the titanium alloy is Ti-6Al-4V, Ti-6Al-6V-2Sn, Ti-6Al-2Sn-4Zr-6Mo, Ti-10V-2Fe-3Al, Ti-7Al-4Mo and Ti-13V-11Cr- It may be selected from commercial titanium alloys such as 3Al.

In addition, the deoxidizer may use calcium.

In addition, the washing may be carried out by one or more methods of water washing and acid washing.

Drying may also be carried out by vacuum drying.

In the method for preparing low oxygen titanium alloy powder according to the present invention, deoxidation is performed at 950-1050 ° C. for 1 to 3 hours using 80 to 120 parts by weight of a deoxidizer based on 100 parts by weight of the titanium alloy mother powder.

As a result, a low oxygen titanium alloy powder having an oxygen content of 2000 ppm by weight or less can be produced.

Figure 1 schematically shows a method for producing a low oxygen titanium alloy powder according to an embodiment of the present invention.
Figure 2 schematically shows a device that can be used to produce a low oxygen titanium alloy powder according to the present invention.

Advantages and features of the present invention and methods for achieving them will be apparent with reference to the embodiments described below in detail with the accompanying drawings. It should be understood, however, that the invention is not limited to the disclosed embodiments, but is capable of many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, To fully disclose the scope of the invention to those skilled in the art, and the invention is only defined by the scope of the claims. Like reference numerals refer to like elements throughout the specification.

Hereinafter, a method of manufacturing a low oxygen titanium alloy powder according to a preferred embodiment of the present invention will be described in detail with reference to the accompanying drawings.

Figure 1 schematically shows a method for producing a low oxygen titanium alloy powder according to an embodiment of the present invention.

Referring to Figure 1, the method for producing a low oxygen titanium alloy powder according to the present invention includes a titanium alloy powder / deoxidizer placement step (S110), deoxidation step (S120) and washing / drying step (S130).

First, in the titanium alloy hair powder / deoxidizer disposing step (S110), the titanium alloy hair powder and the deoxidizer are separately disposed in the deoxidizing container as shown in FIG. 2. In the present invention, the titanium alloy mother powder and the deoxidizer are disposed separately, because when the titanium alloy mother powder and the deoxidizer are disposed together, it is difficult to separate the deoxidizer after deoxidation by melting the deoxidizer.

Titanium alloys include Ti-6Al-4V, Ti-6Al-6V-2Sn, Ti-6Al-2Sn-4Zr-6Mo, Ti-10V-2Fe-3Al, Ti-7Al-4Mo, Ti-13V-11Cr-3Al, etc. Can be.

The deoxidation container includes a lower container 220a and an upper container 220b. The lower container 220a has an open top, and a deoxidizer is disposed. The upper container 220b is coupled onto the lower container 220a, and a titanium alloy mother powder is disposed. At this time, the lower surface of the upper vessel 220b is a sieve 240, so that the deoxidizer evaporated in the lower vessel 220a passes through the sheave so that the titanium alloy hair powder is deoxidized.

On the other hand, when the inside of the lower container 220a is heated above the melting temperature of the deoxidizer, the deoxidizer is melted, and in this case, it is difficult to completely remove the deoxidizer adhering to the inside of the lower container by solidifying after using the deoxidizer. Therefore, reuse of the lower container 220a may be difficult. In order to solve this problem, it is more preferable to use a disposable deoxidant storage cup 230 mounted in the lower container 220a and directly storing the deoxidant.

On the other hand, the deoxidizer is preferably used at 80 to 120 parts by weight with respect to 100 parts by weight of the titanium alloy mother powder. When the amount of the deoxidizer is less than 80 parts by weight relative to 100 parts by weight of the titanium alloy mother powder, the deoxidation effect is insufficient. On the contrary, when the amount of the deoxidizer exceeds 120 parts by weight based on 100 parts by weight of the titanium alloy mother powder, only the amount of the deoxidizer may be increased without further deoxidation effect.

Next, in the deoxidation step (S120), next, in the deoxidation step (S120) by heating the inside of the lower vessel 220a and the upper vessel 220b to 950 ~ 1050 ℃, using deoxidizer evaporation for 1 to 3 hours under vacuum To deoxidize the titanium alloy powder. Deoxidation is a process in which the deoxidizer comes into contact with the titanium alloy powder as the deoxidizer evaporates, whereby oxygen (O) contained in the titanium alloy powder is chemically reacted with the deoxidizer.

At this time, the deoxidation is preferably carried out for 1 to 3 hours at 950 ~ 1050 ℃. When the deoxidation temperature is less than 950 ° C. or the deoxidation holding time is less than 1 hour, deoxidation is insufficient and it is difficult to obtain a low oxygen titanium alloy powder having a target oxygen content of 2000 ppm by weight or less. On the contrary, when the deoxidation temperature exceeds 1050 ° C. or the deoxidation time exceeds 3 hours, it is difficult to completely remove deoxidation by-products such as CaO after deoxidation due to sintering and agglomeration of the titanium alloy powder.

Next, in the washing / drying step (S130), the deoxidized titanium alloy powder is washed to remove deoxidation by-products such as calcium oxide on the surface of the deoxidized titanium alloy powder, and then dried to obtain a final titanium alloy powder.

The washing can be carried out by one or more methods of water washing and acid washing. For acid washes, approximately 10% by weight HCl solution can be used. In order to obtain a low oxygen titanium alloy powder, it is more preferable to repeat the water washing and the acid washing several times.

The drying may be carried out in various ways, but more preferably carried out by vacuum drying to obtain a low oxygen titanium alloy powder. Vacuum drying may be carried out at approximately 60 ° C. for about 2 hours.

Example

Hereinafter, a method of manufacturing a low oxygen titanium alloy powder according to the present invention will be described through a preferred embodiment of the present invention. It is to be understood, however, that the same is by way of illustration and example only and is not to be construed in a limiting sense.

Details that are not described herein will be omitted since those skilled in the art can sufficiently infer technically.

1. Experiment apparatus

For this experiment, a deoxidation device specially manufactured as shown in FIG. 2 was used.

The outer container 210 is for preventing leakage of the evaporated deoxidizer (calcium), the material of which is steel. The inner container 220 is composed of a lower container 220a, an upper container 220b, and a coupling portion 220c for fastening the lower container 220a and the upper container 220b, and the material of each part is made of steel. It was.

The upper container 220a is loaded with titanium alloy mother powder 201 and has a shape in which a sheave 240 is coupled to a lower portion thereof. In addition, the edge was fixed with a gasket so that the sheave 240 did not move. In addition, the sheave 240 was made of 150 mesh so that the titanium alloy mother powder 201 did not fall. The lower vessel 220b is designed to evaporate the deoxidizer from the high temperature to the upper direction, and used a disposable deoxidizer storage cup 230 for reuse of the lower vessel 220b. After the inner container 220 is disposed, the deoxidation container is sealed using the inner container cover 221 and the outer container cover 211.

2. Preparation of Titanium Alloy Powder

Ti-6Al-4V powder containing 3,870 ppm by weight of oxygen was used as the titanium alloy mother powder. The deoxidizer used calcium in the same amount as Ti-6Al-4V. Deoxidation was carried out for 2 hours under the conditions shown in Table 1 under a vacuum of 1 × 10 ⁻⁵ torr.

Thereafter, the deoxidized Ti-6Al-4V powder was repeatedly washed three times with water and acid wash (10 wt% HCl solution), followed by vacuum drying at 60 ° C. for 2 hours to obtain Ti-6Al-4V powder.

[Table 1]

3. Oxygen content measurement

Thereafter, after deoxidation, the oxygen content of Ti-6Al-4V powders according to specimens 1 to 6 was measured using an oxygen / nitrogen analyzer (LECO TCH-600).

Referring to Table 1, in the case of specimen 2 satisfying the conditions given in the present invention according to the deoxidation temperature, the oxygen content was 2,000 ppm by weight or less.

On the other hand, for specimen 1, which has a relatively low deoxidation temperature of 900 ° C., the oxygen content exceeded 2,000 ppm by weight, because deoxidation of the Ti-6Al-4V powder requires a higher temperature.

In the case of specimen 3, which has a relatively high deoxidation temperature of 1100 ° C, the oxygen content exceeded 3,000 ppm by weight, because the Ti-6Al-4V powder was agglomerated with calcium and CaO was not completely removed after deoxidation. .

While the present invention has been particularly shown and described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. Such changes and modifications are intended to fall within the scope of the present invention unless they depart from the scope of the present invention. Accordingly, the scope of the present invention should be determined by the following claims.

S110: Titanium Alloy Chip Powder / Calcium Batch Step
S120 deoxidation step
S130: washing / drying step
201: titanium alloy powder 202: deoxidizer
210: outer container 211: outer container cover
220: inner container 220a: lower container
220b: upper container 220c: coupling portion
221: inner container cover 230: deoxidant storage cup
240: sheave

Claims (5)

(a) placing 80 to 120 parts by weight of a deoxidizer in a lower vessel with an open top, and having at least 3,000 ppm by weight of oxygen on the sheave of the upper vessel coupled to the lower vessel and having a bottom surface sieve; Arranging 100 parts by weight of a titanium alloy powder comprising;
(b) heating the lower vessel and the upper vessel to 950-1050 ° C. to deoxidize the titanium alloy powder using the deoxidizer evaporation for 1-3 hours under a vacuum of 1 × 10 ⁻⁵ torr; And
(c) washing the deoxidized titanium alloy powder and then drying the powder;
The titanium alloy mother powder is Ti-6Al-4V,
Method for producing a low oxygen titanium alloy powder, characterized in that the oxygen content of the titanium alloy powder obtained in step (c) is 1,760 to 2,000 ppm by weight.
delete The method of claim 1,
In step (c), washing
A method for producing low oxygen titanium alloy powder, characterized in that it is carried out by at least one method of water washing and acid washing.
The method of claim 1,
In the step (c), drying
A method for producing a low oxygen titanium alloy powder, characterized in that it is carried out by vacuum drying.
A low oxygen titanium alloy powder prepared by the method according to any one of claims 1, 3 and 4, having an oxygen content of 1,760 to 2,000 ppm by weight.

Images