CN116399667A - A kind of dissolving method of germanium tellurium antimony alloy - Google Patents

Abstract

The invention relates to a dissolving method of germanium tellurium antimony alloy, which comprises the following steps: the germanium tellurium antimony alloy and the mixed acid are subjected to first mixing to obtain mixed liquid, and then hydrofluoric acid is added into the mixed liquid to perform second mixing to obtain solution; the mixed acid comprises hydrochloric acid and nitric acid with the volume ratio of (1-2) being 1. According to the dissolving method provided by the invention, through adopting a specific dissolving process for the germanium tellurium antimony alloy, firstly, mixed acid is used for dissolving to obtain clear and transparent solution, and then a certain amount of hydrofluoric acid is added to enhance the stability of the solution and improve the detection sensitivity of the solution.

Description

A kind of dissolving method of germanium tellurium antimony alloy

technical field

The invention relates to the field of sample detection, in particular to a method for dissolving germanium tellurium antimony alloy.

Background technique

At present, germanium tellurium antimony alloy is a typical phase change material, and the reflectivity and resistivity corresponding to the crystalline and amorphous structures of the thin film are very different, so it is widely used in the field of information storage.

For example, CN114635109A discloses a sputtering target and a method for manufacturing electronic devices using the sputtering target. The sputtering target may comprise a carbon-doped GeSbTe alloy, wherein, for the carbon-doped GeSbTe alloy, the average particle size of the sintered GeSbTe alloy is in the range of 0.5 μm to 5 μm, and the average particle size of the sintered carbon is Y μm The first ratio with respect to the average grain diameter of the sintered GeSbTe alloy may be in a range of greater than 0.5 and less than or equal to 1.5. Optionally, for the carbon-doped GeSbTe alloy, the condition of Y=X×(Z/100) can be satisfied, wherein the average particle size of the sintered GeSbTe alloy is X μm, and the average particle size of the sintered carbon is Y μm , and the carbon content is Zat%.

_CN112719278A A method for preparing _{germanium -} antimony-tellurium alloy powder, comprising steps _: step 1, preparing germanium, antimony _{, tellurium simple} substances, germanium, The purity of antimony and tellurium is more than 4.5N. Vacuum melting of germanium, antimony and tellurium to form a molten mixture, using high-pressure inert gas to atomize and condense the molten mixture to retain the high-temperature phase, to obtain Ge ₂ Sb ₂ Te with a particle size of less than 45 microns _5. GeSb ₂ Te ₄ or GeSb ₄ Te ₇ germanium antimony tellurium alloy powder; step 2, subjecting the germanium antimony tellurium alloy powder obtained in step 1 to jet milling; step 3, subjecting the germanium antimony tellurium alloy powder pulverized in step 2 to Classify by air flow to obtain germanium antimony tellurium powder with D90 less than 10 microns. The present disclosure adopts the gas atomization method, the cooling speed of the alloy liquid is fast, the segregation of the structure is avoided, and it becomes a single phase, and the Ge ₂ Sb ₂ Te ₅ , GeSb ₂ Te ₄ or GeSb ₄ Te with a particle size of less than 45 microns is obtained in the gas atomization After ₇ , use the brittleness of Ge ₂ Sb ₂ Te ₅ , GeSb ₂ Te ₄ or GeSb ₄ Te ₇ to obtain germanium antimony tellurium powder with D90 less than 10 through jet milling and jet classification.

However, after the current germanium tellurium antimony alloy is prepared, it usually needs to be tested to confirm its composition. The detection of the alloy is usually carried out by inductively coupled plasma emission spectrometer. The sample needs to be dissolved before the test, but for the germanium tellurium antimony alloy The dissolution still has the problem that solids will precipitate out after a period of time after dissolution, and the dissolution effect is poor.

Contents of the invention

In view of the problems existing in the prior art, the object of the present invention is to provide a method for dissolving germanium tellurium antimony alloy, so as to solve the problem of poor dissolution effect due to the precipitation of solids after a period of time after the complete dissolution of germanium tellurium antimony alloy.

For reaching this purpose, the present invention adopts following technical scheme:

The invention provides a kind of dissolving method of germanium tellurium antimony alloy, and described dissolving method comprises:

The germanium tellurium antimony alloy is first mixed with the mixed acid to obtain a mixed solution, and then hydrofluoric acid is added to the mixed solution for the second mixing to obtain a solution;

The mixed acid includes hydrochloric acid and nitric acid with a volume ratio of (1-2):1.

The dissolving method provided by the present invention adopts a specific dissolving process for germanium tellurium antimony alloy, first dissolves into a clear and transparent solution by mixed acid, and then adds a certain amount of hydrofluoric acid to enhance the stability of the solution and improve the solution. detection sensitivity.

In the present invention, the mixed acid includes hydrochloric acid and nitric acid with a volume ratio of (1-2):1, such as 1:1, 1.05:1, 1.1:1, 1.15:1, 1.2:1, 1.25:1 , 1.3:1, 1.35:1, 1.4:1, 1.45:1, 1.5:1, 1.55:1, 1.6:1, 1.65:1, 1.7:1, 1.75:1, 1.8:1, 1.85:1, 1.9 :1, 1.95:1 or 2:1, etc., but not limited to the listed values, other unlisted values within this range are also applicable.

As a preferred technical solution of the present invention, the germanium-tellurium-antimony alloy comprises, in terms of mass percentage, 14-15% germanium, 61-63% tellurium, and the balance is antimony.

In the present invention, the germanium in the germanium tellurium antimony alloy is 14-15% by mass, such as 14%, 14.1%, 14.2%, 14.3%, 14.4%, 14.5%, 14.6%, 14.7% %, 14.8%, 14.9% or 15%, etc., but not limited to the listed values, other unlisted values within this range are also applicable.

In the present invention, the tellurium in the germanium-tellurium-antimony alloy is 61-63% by mass, for example, 61%, 61.1%, 61.2%, 61.3%, 61.4%, 61.5%, 61.6%, 61.7% %, 61.8%, 61.9%, 62%, 62.1%, 62.2%, 62.3%, 62.4%, 62.5%, 62.6%, 62.7%, 62.8%, 62.9% or 63%, but not limited to the listed values, the Other unrecited values within the range also apply.

As a preferred technical solution of the present invention, the solid-to-liquid ratio g/mL in the first mixing is 1:(30-50), such as 1:30, 1:31, 1:32, 1:33, 1 :34, 1:35, 1:36, 1:37, 1:38, 1:39, 1:40, 1:41, 1:42, 1:43, 1:44, 1:45, 1:46 , 1:47, 1:48, 1:49 or 1:50, etc., but not limited to the listed values, other unlisted values within this range are also applicable.

As a preferred technical solution of the present invention, the holding temperature in the first mixing is 80-100°C, such as 80°C, 81°C, 82°C, 83°C, 84°C, 85°C, 86°C, 87°C, 88°C, 89°C, 90°C, 91°C, 92°C, 93°C, 94°C, 95°C, 96°C, 97°C, 98°C, 99°C or 100°C, etc., but not limited to the listed values, within this range Other values not listed also apply.

As a preferred technical solution of the present invention, the first mixing time is 15-30min, such as 15min, 15.5min, 16min, 16.5min, 17min, 17.5min, 18min, 18.5min, 19min, 19.5min, 20min, 20.5min, 21min, 21.5min, 22min, 22.5min, 23min, 23.5min, 24min, 24.5min or 25min, etc., but not limited to the listed values, other unlisted values within this range are also applicable.

As a preferred technical solution of the present invention, the amount of hydrofluoric acid added in the second mixing is 10-12 times the mass of the germanium tellurium antimony alloy, for example, it can be 10 times, 10.1 times, 10.2 times, 10.3 times, 10.4 times, 10.5 times, 10.6 times, 10.7 times, 10.8 times, 10.9 times, 11 times, 11.1 times, 11.2 times, 11.3 times, 11.4 times, 11.5 times, 11.6 times, 11.7 times, 11.8 times, 11.9 times or 12 times, etc., but Not limited to the listed values, other unlisted values within this range are also applicable.

As a preferred technical solution of the present invention, the holding temperature in the second mixing is 90-100°C, such as 90°C, 91°C, 92°C, 93°C, 94°C, 95°C, 96°C, 97°C, 98°C, 99°C, or 100°C, etc., but not limited to the listed values, and other unlisted values within this range are also applicable.

As a preferred technical solution of the present invention, the second mixing time is 10-25min, such as 10min, 10.5min, 11min, 11.5min, 12min, 12.5min, 13min, 13.5min, 14min, 14.5min, 15min, 15.5min, 16min, 16.5min, 17min, 17.5min, 18min, 18.5min, 19min, 19.5min, 20min, 20.5min, 21min, 21.5min, 22min, 22.5min, 23min, 23.5min, 24min, 24.5min or 25min, etc. , but not limited to the listed values, other unlisted values within this range are also applicable.

As a preferred technical solution of the present invention, the hydrochloric acid is concentrated hydrochloric acid.

In the present invention, the concentrated hydrochloric acid is analytically pure concentrated hydrochloric acid with a mass concentration of 35-37%.

Preferably, the nitric acid is concentrated nitric acid.

In the present invention, the concentrated nitric acid is analytically pure concentrated nitric acid with a mass concentration greater than or equal to 68%.

Preferably, the mass concentration of the hydrofluoric acid is 37-42%, such as 37%, 37.2%, 37.4%, 37.6%, 37.8%, 38%, 38.2%, 38.4%, 38.6%, 38.8%, 39%, 39.2%, 39.4%, 39.6%, 39.8%, 40%, 40.2%, 40.4%, 40.6%, 40.8%, 41%, 41.2%, 41.4%, 41.6%, 41.8%, or 42%, etc., but Not limited to the listed values, other unlisted values within this range are also applicable.

In the present invention, the reagents are analytically pure reagents.

As a preferred technical solution of the present invention, the dissolution method includes:

The germanium tellurium antimony alloy is first mixed with the mixed acid to obtain a mixed solution, and then hydrofluoric acid is added to the mixed solution for the second mixing to obtain a solution;

The germanium-tellurium-antimony alloy includes, in terms of mass percentages: 14-15% germanium, 61-63% tellurium, and the balance is antimony; the mixed acid includes hydrochloric acid and Nitric acid; the solid-to-liquid ratio g/mL in the first mixing is 1:(30-50); the insulation temperature in the first mixing is 80-100°C; the first mixing time is 15-30min ; The amount of hydrofluoric acid added in the second mixing is 10-12 times of the quality of the germanium tellurium antimony alloy; the heat preservation temperature in the second mixing is 90-100 °C; the time of the second mixing is 10- 25min; the hydrochloric acid is concentrated hydrochloric acid; the nitric acid is concentrated nitric acid; the mass concentration of the hydrofluoric acid is 37-42%.

Compared with the prior art solutions, the present invention has the following beneficial effects:

The dissolution method provided by the present invention ensures the long-term stability of the solution by adopting a specific dissolution process, and improves the detection sensitivity of inductively coupled plasma emission detection.

Detailed ways

For better illustrating the present invention, facilitate understanding technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:

Example 1

This embodiment provides a kind of dissolving method of germanium tellurium antimony alloy, and described dissolving method comprises:

The germanium tellurium antimony alloy is first mixed with the mixed acid to obtain a mixed solution, and then hydrofluoric acid is added to the mixed solution for the second mixing to obtain a solution;

The content of the germanium-tellurium-antimony alloy in terms of mass percentage is: germanium 14.15%, tellurium 62.13%, and the balance is antimony;

The mixed acid includes hydrochloric acid and nitric acid with a volume ratio of 1:1; the solid-to-liquid ratio g/mL in the first mixing is 1:40; the holding temperature in the first mixing is 90°C; The mixing time is 23min;

The amount of hydrofluoric acid added in the second mixing is 11 times the mass of the germanium tellurium antimony alloy; the holding temperature in the second mixing is 95°C; the time of the second mixing is 15 minutes; the hydrochloric acid is concentrated Hydrochloric acid (mass concentration is 37%); described nitric acid is concentrated nitric acid (mass concentration is 68%); The mass concentration of described hydrofluoric acid is 40%.

Example 2

This embodiment provides a kind of dissolving method of germanium tellurium antimony alloy, and described dissolving method comprises:

The germanium tellurium antimony alloy is first mixed with the mixed acid to obtain a mixed solution, and then hydrofluoric acid is added to the mixed solution for the second mixing to obtain a solution;

The germanium-tellurium-antimony alloy includes, by mass percentage: 14% germanium, 63% tellurium, and the balance is antimony;

The mixed acid includes hydrochloric acid and nitric acid with a volume ratio of 1.5:1; the solid-to-liquid ratio g/mL in the first mixing is 1:30; the holding temperature in the first mixing is 80°C; the second mixing The mixing time is 30min;

The amount of hydrofluoric acid added in the second mixing is 12 times the mass of the germanium tellurium antimony alloy; the holding temperature in the second mixing is 90°C; the time of the second mixing is 12 minutes; the hydrochloric acid is concentrated Hydrochloric acid (mass concentration is 37%); described nitric acid is concentrated nitric acid (mass concentration is 68%); The mass concentration of described hydrofluoric acid is 37%.

Example 3

This embodiment provides a kind of dissolving method of germanium tellurium antimony alloy, and described dissolving method comprises:

The germanium tellurium antimony alloy is first mixed with the mixed acid to obtain a mixed solution, and then hydrofluoric acid is added to the mixed solution for the second mixing to obtain a solution;

The germanium-tellurium-antimony alloy includes, in terms of mass percentage, 15% germanium, 61% tellurium, and the balance is antimony;

The mixed acid includes hydrochloric acid and nitric acid with a volume ratio of 1.8:1; the solid-to-liquid ratio g/mL in the first mixing is 1:50; the holding temperature in the first mixing is 100°C; The mixing time is 15min;

The amount of hydrofluoric acid added in the second mixing is 10 times the mass of germanium tellurium antimony alloy; the holding temperature in the second mixing is 100°C; the time of the second mixing is 25min; the hydrochloric acid is concentrated Hydrochloric acid (mass concentration is 37%); described nitric acid is concentrated nitric acid (mass concentration is 68%); The mass concentration of described hydrofluoric acid is 42%.

Example 4

This embodiment provides a kind of dissolving method of germanium tellurium antimony alloy, and described dissolving method comprises:

The germanium tellurium antimony alloy is first mixed with the mixed acid to obtain a mixed solution, and then hydrofluoric acid is added to the mixed solution for the second mixing to obtain a solution;

The germanium-tellurium-antimony alloy includes, in terms of mass percentage, 14.61% germanium, 61.84% tellurium, and the balance is antimony;

The mixed acid includes hydrochloric acid and nitric acid with a volume ratio of 2:1; the solid-to-liquid ratio g/mL in the first mixing is 1:45; the holding temperature in the first mixing is 100°C; The mixing time is 30min;

The amount of hydrofluoric acid added in the second mixing is 12 times the mass of germanium tellurium antimony alloy; the holding temperature in the second mixing is 100°C; the time of the second mixing is 25min; the hydrochloric acid is concentrated Hydrochloric acid (mass concentration is 37%); described nitric acid is concentrated nitric acid (mass concentration is 68%); The mass concentration of described hydrofluoric acid is 38%.

Example 5

The difference from Example 1 is only that hydrochloric acid is replaced by sulfuric acid of equal concentration.

Example 6

The difference with embodiment 1 is only that nitric acid is changed into the sulfuric acid of equal concentration.

Example 7

The difference from Example 1 is only that hydrofluoric acid is replaced by hydrofluoric acid of equal concentration.

Example 8

The difference from Example 1 is only that the hydrofluoric acid in the second mixing is replaced by sulfuric acid of equal concentration.

Example 9

The difference from Example 1 is only that the hydrofluoric acid in the second mixing is replaced by nitric acid of equal concentration.

The solution obtained in Examples 1-9 was diluted to meet the detection requirements on the machine, and was detected by an inductively coupled plasma emission spectrometer (Agilent 5110). The analysis of the detection results is shown in Table 1.

Table 1

It can be known from the results of the above examples that the dissolution method provided by the present invention adopts a specific dissolution process for the germanium tellurium antimony alloy, first dissolves into a clear and transparent solution by mixed acid, and then adds a certain amount of hydrofluoric acid to strengthen the solution. Stability, and improve the detection sensitivity of the solution.

It is stated that the present invention illustrates the detailed structural features of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned detailed structural features, that is, it does not mean that the present invention must rely on the above-mentioned detailed structural features to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of selected components in the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the scope of protection and disclosure of the present invention.

The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solutions of the present invention. These simple modifications All belong to the protection scope of the present invention.

In addition, it should be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable way if there is no contradiction. The combination method will not be described separately.

In addition, various combinations of different embodiments of the present invention can also be combined arbitrarily, as long as they do not violate the idea of the present invention, they should also be regarded as the disclosed content of the present invention.

Claims (10)

1. a dissolving method of germanium tellurium antimony alloy, is characterized in that, described dissolving method comprises: The germanium tellurium antimony alloy is first mixed with the mixed acid to obtain a mixed solution, and then hydrofluoric acid is added to the mixed solution for the second mixing to obtain a solution; The mixed acid includes hydrochloric acid and nitric acid with a volume ratio of (1-2):1. 2 . The dissolving method according to claim 1 , wherein the germanium tellurium antimony alloy comprises, by mass percentage: 14-15% germanium, 61-63% tellurium, and the balance is antimony. 3. dissolving method as claimed in claim 1 or 2, is characterized in that, the solid-liquid ratio g/mL in the first mixing is 1:(30-50). 4. The dissolution method according to any one of claims 1-3, characterized in that, the holding temperature in the first mixing is 80-100°C. 5. The dissolving method according to any one of claims 1-4, characterized in that, the first mixing time is 15-30min. 6. The dissolving method according to any one of claims 1-5, characterized in that the amount of hydrofluoric acid added in the second mixing is 10-12 times the mass of the germanium tellurium antimony alloy. 7. The dissolution method according to any one of claims 1-6, characterized in that, the holding temperature in the second mixing is 90-100°C. 8. The dissolving method according to any one of claims 1-7, characterized in that, the second mixing time is 10-25min. 9. as described in any one of claim 1-8 dissolving method, it is characterized in that, described hydrochloric acid is concentrated hydrochloric acid; Preferably, the nitric acid is concentrated nitric acid; Preferably, the mass concentration of the hydrofluoric acid is 37-42%. 10. The dissolving method according to any one of claims 1-9, wherein the dissolving method comprises: The germanium tellurium antimony alloy is first mixed with the mixed acid to obtain a mixed solution, and then hydrofluoric acid is added to the mixed solution for the second mixing to obtain a solution; The germanium-tellurium-antimony alloy includes, in terms of mass percentages: 14-15% germanium, 61-63% tellurium, and the balance is antimony; the mixed acid includes hydrochloric acid and Nitric acid; the solid-to-liquid ratio g/mL in the first mixing is 1:(30-50); the insulation temperature in the first mixing is 80-100°C; the first mixing time is 15-30min ; The amount of hydrofluoric acid added in the second mixing is 10-12 times of the quality of the germanium tellurium antimony alloy; the heat preservation temperature in the second mixing is 90-100 °C; the time of the second mixing is 10- 25min; The hydrochloric acid is concentrated hydrochloric acid; the nitric acid is concentrated nitric acid; the mass concentration of the hydrofluoric acid is 37-42%.