阅读说明：本技术 一种高纯银蒸发料的制备方法 (Preparation method of high-purity silver evaporation material ) 是由 姚力军 边逸军 潘杰 王学泽 汪焱斌 慕二龙 于 2021-01-29 设计创作，主要内容包括：本发明涉及一种高纯银蒸发料的制备方法,所述制备方法包括以下步骤：(1)将高纯银锭和挤压模具经预热后进行挤压作业,得到直径为8-10mm的中间料；(2)将中间料进行拉拔处理,得到直径为3-6mm的所述高纯银蒸发料。本发明提供的制备方法,通过采用将挤压作业和拉拔处理相结合,并控制挤压作业产品的直径,以保证拉拔时具有特定的进料直径,并控制最终高纯银蒸发料产品的直径实现了高性能银蒸发料的制备,使得其作为银蒸发料镀膜时具有致密度高,组织均匀分布的特性。(The invention relates to a preparation method of a high-purity silver evaporation material, which comprises the following steps: (1) preheating a high-purity silver ingot and an extrusion die and then carrying out extrusion operation to obtain an intermediate material with the diameter of 8-10 mm; (2) and drawing the intermediate material to obtain the high-purity silver evaporation material with the diameter of 3-6 mm. The preparation method provided by the invention combines the extrusion operation and the drawing treatment, controls the diameter of the product of the extrusion operation to ensure that the product has a specific feeding diameter during drawing, and controls the diameter of the final high-purity silver evaporation material product to realize the preparation of the high-performance silver evaporation material, so that the silver evaporation material has the characteristics of high density and uniform tissue distribution when being used as a silver evaporation material for coating.)

1. The preparation method of the high-purity silver evaporation material is characterized by comprising the following steps of:

(1) preheating a high-purity silver ingot and an extrusion die and then carrying out extrusion operation to obtain an intermediate material with the diameter of 8-10 mm;

(2) and drawing the intermediate material to obtain the high-purity silver evaporation material with the diameter of 3-6 mm.

2. The method as set forth in claim 1, wherein the preheating temperature in step (1) is 600-800 ℃.

3. The method as set forth in claim 1 or 2, wherein the extrusion force in the extrusion operation in the step (1) is 4000- > 5000 kN.

4. The production method according to any one of claims 1 to 3, wherein the extrusion rate of the extrusion operation of the step (1) is 3 to 8 mm/s.

5. The method according to claim 4, wherein the extrusion rate of the extrusion operation of the step (1) is 5 to 6 mm/s.

6. The production method according to any one of claims 1 to 5, wherein the single-pass reduction in drawing in the drawing treatment of step (2) is 15 to 30%.

7. The manufacturing method according to claim 6, wherein the drawing single-pass reduction rate in the drawing process of the step (2) is 20-25%.

8. The production method according to any one of claims 1 to 7, wherein the drawing speed in the drawing treatment of the step (2) is 30 to 50 m/min.

9. The production method according to any one of claims 1 to 8, wherein the high purity silver evaporant having a diameter of 3 to 6mm is obtained after straightening after the drawing treatment in the step (2).

10. The method of any one of claims 1 to 9, comprising the steps of:

(1) preheating a high-purity silver ingot and an extrusion die and then carrying out extrusion operation to obtain an intermediate material with the diameter of 8-10 mm; the preheating temperature is 600-800 ℃; the extrusion force in the extrusion operation is 4000- & lt5000 kN-; the extrusion rate of the extrusion operation is 3-8 mm/s;

(2) drawing the intermediate material to obtain the high-purity silver evaporation material with the diameter of 3-6 mm; the single-pass compression rate of drawing in the drawing treatment is 15-30%; the drawing speed in the drawing treatment is 30-50 m/min.

Technical Field

The invention relates to the field of vacuum coating, in particular to a preparation method of a high-purity silver evaporation material.

Background

At present, with the rapid development of the fields such as 5G, cloud computing, artificial intelligence and the like, the chip industry plays a crucial role as a core unit in these fields. Human beings have undergone agricultural revolution, industrial revolution, and information revolution is currently underway. The rapid development of information technology has greatly promoted the development of the integrated circuit industry, and the demand of various countries around the world for chips is increasing day by day.

For example, CN202530153U discloses a new structure of evaporation material for electron beam evaporation coating. The end face of the block-shaped evaporation material directly heated by the electron beam is provided with a groove with a certain size and a certain shape, when the evaporation material is used, the evaporation material in the shape of a sheet or a particle and the material is put into the groove to be melted and evaporated together, so that the splashing of the melt of the evaporation material of the traditional frustum at the beginning of evaporation can be effectively reduced, the melt in the evaporation process is prevented from overflowing, the evaporation material can be applied to the evaporation material of all materials commonly used at present, and the evaporation coating quality is favorably improved.

CN103966554A discloses a vacuum evaporation device and a vacuum evaporation method, the vacuum evaporation device includes: a guide passage for conveying an evaporation material obtained by using the evaporation source; and a releasing member that releases the evaporation material flowing from the guide passage to the evaporation target member. The release member includes: a dispersion vessel (7) for diffusing the evaporation material; and a plurality of nozzle members (8) which are provided so as to protrude toward the member to be vapor-deposited and have, at the tip thereof, a constricted opening for releasing the evaporation material toward the member to be vapor-deposited. Each nozzle member (8) has an inner diameter (D) of the nozzle member (8), a length (L) of the nozzle member (8), and a diameter (D') of the constricted opening (8 a). The release member has a device (13) for adjusting the flow rate of the evaporation material of each nozzle member (8) so that the flow rate of the evaporation material of each nozzle member (8) becomes a predetermined value. The inner diameter (D, mm) of the nozzle member (8), the length (L, mm) of the nozzle member (8), and the diameter (D', mm) of the constricted opening portion satisfy the relation: l is more than or equal to 9D and D 'is less than or equal to 2.7D2/L, or L is less than 9D and D' is less than or equal to D/3.

However, due to the high degree of sophistication and sophistication of the semiconductor industry, the throughput is very limited. The existing process has low production efficiency, particularly high-purity silver (more than or equal to 4N) evaporation materials, the efficiency for preparing the evaporation materials is low, and the performance of the evaporation materials is not low due to the poor process stability, so that the evaporation materials are boiled violently during use, the evaporation materials are splashed seriously, and wafers are damaged.

Disclosure of Invention

In view of the problems in the prior art, the present invention aims to provide a method for preparing a high purity silver evaporation material, so that the prepared high purity silver evaporation material has good evaporation performance, the silver evaporation material does not splash during evaporation, and an obtained coating film has the characteristics of high density and uniform tissue distribution.

In order to achieve the purpose, the invention adopts the following technical scheme:

the invention provides a preparation method of a high-purity silver evaporation material, which comprises the following steps:

(1) preheating a high-purity silver ingot and an extrusion die and then carrying out extrusion operation to obtain an intermediate material with the diameter of 8-10 mm;

(2) and drawing the intermediate material to obtain the high-purity silver evaporation material with the diameter of 3-6 mm.

The preparation method provided by the invention combines the extrusion operation and the drawing treatment, controls the diameter of the product of the extrusion operation to ensure that the product has a specific feeding diameter during drawing, and controls the diameter of the final high-purity silver evaporation material product to realize the preparation of the high-performance silver evaporation material, so that the silver evaporation material has the characteristics of high density and uniform tissue distribution when being used as a silver evaporation material for coating.

In the present invention, the high purity silver ingot has a diameter of 80 to 100mm, for example, 80mm, 82mm, 84mm, 86mm, 88mm, 90mm, 92mm, 94mm, 96mm, 98mm or 100mm, and a height of 300 to 400mm, for example, 300mm, 310mm, 320mm, 330mm, 340mm, 350mm, 360mm, 370mm, 380mm, 390mm or 400mm, but the invention is not limited to the above-mentioned values, and other values not listed in the range are also applicable.

In the present invention, the diameter of the intermediate product is 8 to 10mm, and may be, for example, 8mm, 8.1mm, 8.2mm, 8.3mm, 8.4mm, 8.5mm, 8.6mm, 8.7mm, 8.8mm, 8.9mm, 9mm, 9.1mm, 9.2mm, 9.3mm, 9.4mm, 9.5mm, 9.6mm, 9.7mm, 9.8mm, 9.9mm or 10mm, but not limited to the above-mentioned values, and other values not mentioned in the above-mentioned range are also applicable.

In the present invention, the diameter of the obtained high purity silver evaporant is 3 to 6mm, and may be, for example, 3mm, 3.1mm, 3.2mm, 3.3mm, 3.4mm, 3.5mm, 3.6mm, 3.7mm, 3.8mm, 3.9mm, 4mm, 4.1mm, 4.2mm, 4.3mm, 4.4mm, 4.5mm, 4.6mm, 4.7mm, 4.8mm, 4.9mm, 5mm, 5.1mm, 5.2mm, 5.3mm, 5.4mm, 5.5mm, 5.6mm, 5.7mm, 5.8mm, 5.9mm or 6mm, etc., but is not limited thereto, and other values not specified in the range are also applicable.

As a preferred embodiment of the present invention, the temperature of the preheating in the step (1) is 600 ℃ to 800 ℃, for example, 600 ℃, 610 ℃, 620 ℃, 630 ℃, 640 ℃, 650 ℃, 660 ℃, 670 ℃, 680 ℃, 690 ℃, 700 ℃, 710 ℃, 720 ℃, 730 ℃, 740 ℃, 750 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃ or 800 ℃ and the like, but is not limited to the recited values, and other values not recited in the range are also applicable.

As a preferred embodiment of the present invention, the extrusion pressure in the extrusion operation in the step (1) is 4000-.

As a preferable technical proposal of the invention, the perforation force extrusion rate of the extrusion operation in the step (1) is 3-8mm/s, for example, it may be 3mm/s, 3.2mm/s, 3.4mm/s, 3.6mm/s, 3.8mm/s, 4mm/s, 4.2mm/s, 4.4mm/s, 4.6mm/s, 4.8mm/s, 5mm/s, 5.2mm/s, 5.4mm/s, 5.6mm/s, 5.8mm/s, 6mm/s, 6.2mm/s, 6.4mm/s, 6.6mm/s, 6.8mm/s, 7mm/s, 7.2mm/s, 7.4mm/s, 7.6mm/s, 7.8mm/s, or 8mm/s, etc., but is not limited thereto, and other values not recited in the range may be applied similarly.

According to the invention, the prepared intermediate material has good performance by further regulating and controlling the extrusion force and the extrusion speed in the extrusion operation, the problems of cracks or breakage and the like in the drawing process are avoided, the performance of the coating film obtained when the intermediate material is used as a vapor deposition material is enhanced, and the uniformity of the coating film is further improved.

As a preferable technical scheme of the invention, the extrusion speed of the extrusion operation in the step (1) is 5-6 mm/s.

As a preferable technical proposal of the invention, the single-pass reduction rate of drawing in the drawing treatment of the step (2) is 15-30%.

As a preferable technical proposal of the invention, the single-pass reduction rate of drawing in the drawing treatment of the step (2) is 20-25%.

As a preferable embodiment of the present invention, the drawing speed in the drawing treatment in the step (2) is 30 to 50m/min, and may be, for example, 30m/min, 32m/min, 34m/min, 36m/min, 38m/min, 40m/min, 42m/min, 44m/min, 46m/min, 48m/min or 50m/min, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.

According to the invention, the prepared high-purity silver evaporation material has good performance by further regulating and controlling the single-pass compression ratio and the drawing speed in the drawing treatment, so that the obtained silver evaporation material has good compactness, and the uniformity of the coating film is further improved.

As a preferable technical scheme of the invention, the high-purity silver evaporation material with the thickness of 3-6mm is obtained after straightening after drawing treatment in the step (2). The straightness of the straightened high-purity silver evaporation material is less than or equal to 1.5 mm.

As a preferred technical scheme of the invention, the preparation method comprises the following steps:

(1) preheating a high-purity silver ingot and an extrusion die and then carrying out extrusion operation to obtain an intermediate material with the diameter of 8-10 mm; the preheating temperature is 600-800 ℃; the extrusion force in the extrusion operation is 4000- & lt5000 kN-; the extrusion rate of the extrusion operation is 3-8 mm/s;

(2) drawing the intermediate material to obtain the high-purity silver evaporation material with the diameter of 3-6 mm; the single-pass compression rate of drawing in the drawing treatment is 15-30%; the drawing speed in the drawing treatment is 30-50 m/min.

Compared with the prior art, the invention at least has the following beneficial effects:

(1) the preparation method provided by the invention combines the extrusion operation and the drawing treatment, controls the diameter of the product of the extrusion operation to ensure that the product has a specific feeding diameter during drawing, and controls the diameter of the final high-purity silver evaporation material product to realize the preparation of the high-performance silver evaporation material, so that the silver evaporation material has the characteristics of high density and uniform tissue distribution when being used as a silver evaporation material for coating.

(2) The invention further strengthens the performance of the obtained high-purity silver evaporation material by further regulating and controlling the control parameters in extrusion and drawing, so that the high-purity silver evaporation material has the characteristics of higher density, uniform and more uniformly distributed tissue, and simultaneously avoids the problem of generating cracks or fractures in the drawing process.

Detailed Description

To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:

example 1

The embodiment provides a preparation method of a high-purity silver evaporation material, which comprises the following steps:

(1) preheating a high-purity silver ingot and an extrusion die and then carrying out extrusion operation to obtain an intermediate material with the diameter of 8 mm; the preheating temperature is 700 ℃; the extrusion force in the extrusion operation is 4000 kN; the extrusion rate of the extrusion operation is 5 mm/s;

(2) drawing the intermediate material to obtain the high-purity silver evaporation material with the diameter of 5 mm; the single-pass compression rate of drawing in the drawing treatment is 15 percent; the drawing speed in the drawing treatment was 30 m/min.

The properties of the silver evaporant obtained and the results when used as an evaporant are detailed in table 1.

Example 2

The embodiment provides a preparation method of a high-purity silver evaporation material, which comprises the following steps:

(1) preheating a high-purity silver ingot and an extrusion die and then carrying out extrusion operation to obtain an intermediate material with the diameter of 9 mm; the preheating temperature is 600 ℃; the extrusion force in the extrusion operation is 4500 kN; the extrusion rate of the extrusion operation is 4 mm/s;

(2) drawing the intermediate material to obtain the high-purity silver evaporation material with the diameter of 6 mm; the single-pass compression rate of drawing in the drawing treatment is 20 percent; the drawing speed in the drawing treatment was 40 m/min.

The properties of the silver evaporant obtained and the results when used as an evaporant are detailed in table 1.

Example 3

The embodiment provides a preparation method of a high-purity silver evaporation material, which comprises the following steps:

(1) preheating a high-purity silver ingot and an extrusion die and then carrying out extrusion operation to obtain an intermediate material with the diameter of 10 mm; the preheating temperature is 800 ℃; the extrusion force in the extrusion operation is as follows; the piercing force of the extrusion operation is 5000 kN; the extrusion rate of the extrusion operation is 8 mm/s;

(2) drawing the intermediate material to obtain the high-purity silver evaporation material with the diameter of 4 mm; the single-pass compression rate in the drawing treatment is 30 percent; the drawing speed in the drawing treatment was 50 m/min.

The properties of the silver evaporant obtained and the results when used as an evaporant are detailed in table 1.

Example 4

The embodiment provides a preparation method of a high-purity silver evaporation material, which comprises the following steps:

(1) preheating a high-purity silver ingot and an extrusion die and then carrying out extrusion operation to obtain an intermediate material with the diameter of 8.5 mm; the preheating temperature is 650 ℃; the extrusion force in the extrusion operation is 4800 kN; the extrusion rate of the extrusion operation is 3 mm/s;

(2) drawing the intermediate material to obtain the high-purity silver evaporation material with the diameter of 3 mm; the single-pass compression rate in the drawing treatment is 15 percent; the drawing speed in the drawing treatment was 35 m/min.

The properties of the silver evaporant obtained and the results when used as an evaporant are detailed in table 1.

Example 5

The embodiment provides a preparation method of a high-purity silver evaporation material, which comprises the following steps:

(1) preheating a high-purity silver ingot and an extrusion die and then carrying out extrusion operation to obtain an intermediate material with the diameter of 9.5 mm; the preheating temperature is 750 ℃; the extrusion force in the extrusion operation was 4200 kN; the extrusion rate of the extrusion operation is 7 mm/s;

(2) drawing the intermediate material to obtain the high-purity silver evaporation material with the diameter of 5 mm; the single-pass compression rate in the drawing treatment is 30 percent; the drawing speed in the drawing treatment was 45 m/min.

The properties of the silver evaporant obtained and the results when used as an evaporant are detailed in table 1.

Example 6

The embodiment provides a preparation method of a high-purity silver evaporation material, which comprises the following steps:

(1) preheating a high-purity silver ingot and an extrusion die and then carrying out extrusion operation to obtain an intermediate material with the diameter of 8 mm; the preheating temperature is 700 ℃; the extrusion force in the extrusion operation is 4500 kN; the extrusion rate of the extrusion operation is 6 mm/s;

(2) drawing the intermediate material to obtain the high-purity silver evaporation material with the diameter of 3 mm; the single-pass compression rate in the drawing treatment is 20 percent; the drawing speed in the drawing treatment was 40 m/min.

The properties of the silver evaporant obtained and the results when used as an evaporant are detailed in table 1.

Comparative example 1

The only difference from example 1 is that 5mm silver evaporant was obtained directly by extrusion only, and the properties of the obtained silver evaporant and the results when used as evaporant are shown in table 1. The method has the advantages that thin wires are directly obtained, extrusion force requires high equipment overload, products are too thin and have too high temperature, continuity of silver wires during discharging is reduced, and uniformity of sputtering coating is not facilitated.

Comparative example 2

The difference from example 1 was only that the diameter of the intermediate material after extrusion was controlled to be 12mm, and the properties of the obtained silver evaporant and the results when used as an evaporant were shown in Table 1.

Comparative example 3

The difference from example 1 was only that the extrusion pressure in the extrusion was controlled to 3500kN, and the properties of the obtained silver evaporant and the results when used as an evaporant were shown in Table 1.

Comparative example 4

The difference from example 1 is only that the single-pass reduction rate in drawing was controlled to be 10%, and the properties of the obtained silver evaporant and the results when used as an evaporant are shown in table 1.

Comparative example 5

The difference from example 1 is only that the single-pass reduction rate in drawing was controlled to 40%, and the properties of the obtained silver evaporant and the results when used as an evaporant are shown in table 1. The obtained silver evaporation material has poor performance and can not be plated.

Comparative example 6

The difference from example 1 was only that the drawing speed in drawing was controlled to 60m/min, and the properties of the obtained silver evaporant and the results when used as an evaporant were shown in Table 1. The obtained silver evaporation material has poor performance and can not be plated.

TABLE 1

In the invention, the weak boiling splashing means that the boiling melt does not obviously splash, the middle-finger boiling melt splashes, and the strong-finger boiling melt splashes.

According to the results of the above examples and comparative examples, the preparation method provided by the invention combines the extrusion operation and the drawing treatment, and controls the diameter of the product of the extrusion operation to ensure that the product has a specific feeding diameter during drawing, and controls the diameter of the final high-purity silver evaporation material product to realize the preparation of the high-performance silver evaporation material, so that the silver evaporation material has the characteristics of high density and uniform distribution of tissues when being used as a silver evaporation material coating film.

The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.

It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.

In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.