Silicon powder for thermal spraying and method for manufactruring same

Abstract

The present invention relates to a silicon powder for thermal spraying and a method for manufacturing same and, more specifically, to a silicon powder for thermal spraying, which is used to form a coating layer for realizing wear-resistant, corrosion-resistant, and anti-fouling properties in a device such as a reactor used in a semiconductor manufacturing process, and a method for manufacturing same.

Description

Silicon powder for soldering and method for producing the same

[0001] The present invention relates to a silicon powder for use in a soldering process and a method for producing the same, and more particularly, to a silicon powder for use in a soldering process and a method for producing the same, which is used to form a coating film for implementing wear-resistance, corrosion resistance, and anti-fouling properties in devices such as reactors used in semiconductor manufacturing processes.

[0002] In the field of semiconductor technology, various semiconductor manufacturing process equipment and reactors are required to manufacture semiconductor chips. Examples of these devices include deposition equipment for thin film formation, etching equipment, and photolithography equipment, and each process utilizes a variety of reactors.

[0003] By coating the walls of the reactor in the semiconductor manufacturing process with materials having various properties, the desired function can be imparted.

[0004] Since the semiconductor manufacturing process must maintain a high level of purity, a coating layer is formed on the walls of the reactors to prevent impurities from falling off from the walls of the reactors and contaminating the semiconductor manufacturing materials, and to provide durability to the reactors, which are frequently exposed to highly reactive gas plasma, etc.

[0005] Thermal spraying, a well-known technique for forming a coating film on the walls of a reactor, involves melting and spraying a coating powder. Among the components that can be used in this method, silicon powder is widely used due to its high hardness and wear resistance, excellent thermal stability, excellent corrosion resistance even in harsh environments, and excellent adhesion to various substrates, enabling the formation of a durable coating film.

[0006] At this time, the silicon (Si) powder used as the coating material powder is required to have excellent coating properties and coating uniformity on the reactor wall, exhibit high purity, and have excellent corrosion resistance, wear resistance, and antifouling properties.

[0007] In addition, when manufacturing high-quality silicon powder for soldering, it is common to increase the purity through an additional process such as a refinery, but it is also necessary to develop a method for manufacturing high-purity silicon powder without such a refinery process.

[0008] The purpose of the present invention is to provide a silicon powder for use in a soldering process that can exhibit high purity, excellent coating properties, high corrosion resistance, wear resistance, and antifouling properties when applied as a coating material to the wall surface of a semiconductor manufacturing reactor.

[0009] In addition, the present invention aims to provide a method for manufacturing the silicon powder for use in a soldering iron, which can eliminate an additional purification process and has high yield efficiency and thus high process efficiency.

[0010] The objectives of the present invention are not limited to those mentioned above. Other objectives and advantages of the present invention not mentioned above can be understood through the following description and will be more clearly understood through the embodiments of the present invention. Furthermore, it will be readily apparent that the objectives and advantages of the present invention can be realized by the means and combinations thereof set forth in the claims.

[0011] In order to achieve the above purpose, one aspect of the present invention is D 50 It is possible to provide a silicon powder for soldering, which is 30 to 90 ㎛ in size and has a purity of 99.99% or higher.

[0012] The above-mentioned silicon powder for use as a solder may have a total metal impurity content of 1,000 ppm or less.

[0013] In addition, another aspect of the present invention comprises the steps of: supplying raw material silicon powder to a grinding device; dry grinding the raw material silicon powder in the grinding device; passing the ground silicon powder through a sieve to D 50 A method for producing a silicon powder for soldering can be provided, comprising: a step of selecting a silicon powder satisfying 30 to 90 ㎛; and a step of obtaining a silicon powder for soldering.

[0014] The above-mentioned manufactured silicon powder for soldering may have a purity of 99.99% or higher.

[0015] The above-mentioned manufactured silicon powder for use as a solder may have a total metal impurity content of 1,000 ppm or less.

[0016] The above raw material silicon powder has a total metal impurity content of 500 ppm or less, and D 50 This can be 50 to 200 μm.

[0017] The above grinding device may be any one of a roll mill device, a ball mill device, a jet mill device, and a combination thereof.

[0018] The silicon powder for soldering according to the present invention can exhibit high purity, excellent coatability, and high antifouling properties when applied as a coating material to the wall surface of a semiconductor manufacturing reactor.

[0019] The silicon powder for use in a soldering process according to the present invention can form a silicon thin film on the wall surface of a semiconductor manufacturing reactor by a soldering method, and has a low metal content and excellent corrosion resistance.

[0020] In addition, the method for producing a silicon powder for soldering according to the present invention can eliminate an additional purification process in producing the silicon powder for soldering, thereby increasing process efficiency and obtaining a silicon powder for soldering that exhibits high purity and excellent coatability at a high yield.

[0021] In addition to the effects described above, the effects of the present invention are described together with the description of matters for carrying out the invention below.

[0022] Figure 1 is a schematic diagram illustrating a flow chart of a method for manufacturing a silicon powder for use in a soldering iron according to an example of the present invention.

[0023] Figure 2 shows a PSA analysis graph of a silicon powder for use in a soldering iron according to Example 1 of the present invention.

[0024] Figure 3a shows an SEM image (500x magnification) of a silicon powder for use in a soldering process according to Example 1 of the present invention.

[0025] Figure 3b shows an SEM image (1,000 magnification) of a silicon powder for use in a soldering iron according to Example 1 of the present invention.

[0026] FIG. 4 shows an SEM image of a silicon thin film formed on a glass substrate by plasma spraying using a silicon powder for use in Example 1 of the present invention.

[0027] FIG. 5 shows an EDS image (Energy Dispersive X-Ray Spectrometer Image) of a silicon thin film formed on a glass substrate by plasma spraying using a silicon powder for spraying according to Example 1 of the present invention.

[0028] FIG. 6 shows an EDS image (Energy Dispersive X-Ray Spectrometer Image) of the surface of a silicon thin film formed on a glass substrate by plasma spraying using a silicon powder for spraying according to Example 1 of the present invention.

[0029] The above-described objects, features, and advantages will be described in detail below with reference to the accompanying drawings, so that those skilled in the art can easily practice the technical idea of ​​the present invention. In describing the present invention, if it is determined that a detailed description of known technologies related to the present invention may unnecessarily obscure the gist of the present invention, a detailed description thereof will be omitted. Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the drawings, the same reference numerals are used to indicate the same or similar components.

[0030] In describing this specification, if it is determined that a detailed description of a related known technology may unnecessarily obscure the gist of this specification, the detailed description is omitted.

[0031] In this specification, when the terms "includes," "has," "contains," "arranges," and "provides" are used for a component, other parts may be added, unless "only" is used. When a component is expressed in the singular, it includes the plural unless otherwise explicitly stated.

[0032] In this specification, “thermoplastic powder” means a powder material used for thermal spraying.

[0033] In this specification, "D 50 (Average particle size)" means the average particle size at 50% of the accumulated value in the volume-based particle size distribution measured by a particle size distribution measuring device (PSA) based on laser scattering / diffraction method (50% volume average particle size).

[0034] In interpreting the components in this specification, even if there is no separate explicit description, it is interpreted to include the range of error.

[0035]

[0036] Hereinafter, the present invention will be described in more detail.

[0037]

[0038] The silicon powder for use in the present invention can be usefully used in plasma spraying methods such as atmospheric plasma spraying (APS), low pressure plasma spraying (LPS), and high pressure plasma spraying, and can be used to manufacture a silicon coating thin film.

[0039] When the silicon powder for soldering is formed into a coating film, it must exhibit a uniform and thin coating property, and at the same time, the powder particle size must be controlled for fairness when applied to the soldering method. From this point of view, the D of the silicon powder for soldering of the present invention 50 The D of the silicon powder for use in the present invention may be, for example, 30 to 90 μm, for example, 40 to 80 μm, for example, 50 to 70 μm. 50 If it becomes smaller than the above lower limit, the fluidity is lowered when applied to the spraying method, a uniform coating film cannot be obtained, and the D of the spraying silicon powder of the present invention 50 If it exceeds the above upper limit, a problem may arise in which the melting property of the powder for use as a solder is reduced.

[0040] Meanwhile, due to the metal impurities contained in the silicon powder for soldering, it is difficult to sufficiently implement wear resistance and corrosion resistance, and if impurities are released from the silicon coating film coated on the reactor, it is difficult to obtain excellent antifouling properties. From this point of view, the silicon powder for soldering of the present invention may have a purity of, for example, 99.99% (4N) or higher, for example, 99.999% (5N) or higher, and for example, 99.9999% (6N) or higher.

[0041] The total metal impurity content of the silicon powder for spraying of the present invention may be, for example, 1,000 ppm, for example, 800 ppm or less, for example, 500 ppm, for example, 400 ppm or less, for example, 200 ppm or less, for example, 100 ppm or less, for example, 50 ppm or less. At this time, the content of metal impurities was measured with an 'ICP-OES analyzer' of Thermo Fisher Scientific (the ppm unit of the metal impurity content is based on weight), and the metal elements to be measured may include Al, As, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Sn, Sr, Ti, V, Zn, and Zr.

[0042]

[0043] The silicon powder for soldering of the present invention can be manufactured according to a method for manufacturing silicon powder for soldering, which comprises the following steps.

[0044] (a) a step of supplying raw silicon powder to a grinding device;

[0045] (b) a step of dry-grinding the raw material silicon powder in the grinding device;

[0046] (c) Pass the above crushed silicon powder through a sieve and D 50 A step of selecting silicon powder satisfying 30 to 90 ㎛; and

[0047] (d) A step of obtaining a silicon powder for use as a solder.

[0048]

[0049] In the present invention, in order to obtain high-purity silicon powder for thermal spraying without an additional purification process, a raw silicon powder having high purity, particularly a low metal content, is selected. As the raw silicon powder is pulverized, the content of metal impurities tends to increase due to metal components derived from the pulverizing device. Therefore, it is preferable to select a raw silicon powder having a metal impurity content lower than the target metal impurity content of the final silicon powder for thermal spraying.

[0050] From this point of view, the purity of the raw material silicon powder may be, for example, 500 ppm or less, for example, 300 ppm or less, for example, 200 ppm or less, for example, 100 ppm or less, for example, 80 ppm or less, for example, 50 ppm or less, for example, 30 ppm or less, for example, 20 ppm or less, but is not necessarily limited thereto, and the raw material silicon powder may be selected by considering the target value of the total metal content of the silicon powder for use in the final soldering to be obtained.

[0051] In addition, the raw material silicon powder is used to manufacture the silicon powder for soldering to be obtained as a final product. 50 silver For example, it may be 50 to 200 ㎛, for example, it may be 60 to 150 ㎛, for example, it may be 70 to 100 ㎛, but it is not necessarily limited thereto, and the D of the silicon powder for use in the final soldering to be obtained 50 The raw material silicon powder can be selected by considering the target value.

[0052]

[0053] Then, the raw silicon powder can be ground into a desired particle size through a dry grinding step in the grinding device. The grinding device is not particularly limited, but may be any one of a roll mill device, a ball mill device, a jet mill device, and a combination thereof, but is not limited thereto.

[0054] The above roll mill device is not limited to a roll made of a ceramic material, and may use a roll made of a ceramic material including, for example, alumina, tungsten carbide, zirconia, etc., but is not necessarily limited thereto.

[0055] Afterwards, the above-mentioned crushed silicon powder is passed through a sieve to D 50 The final silicon powder can be obtained by selecting silicon powder satisfying this 30~90 ㎛. The target D 50 You can select and place the body size according to your preference.

[0056] Hereinafter, the present invention will be described in more detail through examples and experimental examples. However, the following examples and experimental examples are merely illustrative of the present invention, and the content of the present invention is not limited to the following examples and experimental examples.

[0057] Example 1

[0058] D 50 A raw silicon powder having a diameter of 90.18 μm and a total metal content of 12 ppm was prepared (OCI). The raw silicon powder was ground in a 2-roll mill (Gap: 0 mm, roll material: alumina) to obtain a silicon powder for use in a spraying machine.

[0059] The obtained silicon powder for soldering was measured three times using a PSA (Particle Size Analyzer) and the average value was plotted and shown in Figure 2, from which D 50 The measurement result was 63.9㎛.

[0060] In addition, the SEM images of the obtained silicon powder for soldering are shown in Figs. 3a and 3b (500x and 1,000x magnifications). The metal content of the obtained silicon powder for soldering was analyzed and shown in Table 1 below.

[0061] A silicon coating thin film was formed on a Pyrex glass substrate by applying a plasma spraying method using argon gas (Ar) as a plasma operating gas to the above-mentioned silicon powder.

[0062] Images of the thickness of the formed silicon coating thin film observed using an SEM device and an EDS device are shown in Figs. 4 to 6. Specifically, Fig. 4 is an SEM image of the surface of the coating thin film, Fig. 5 is an EDS mapping image of the coating thin film, and Fig. 6 shows an EDS image of the surface of the coating thin film.

[0063] As a result of the SEM image analysis of Fig. 4, the average thickness (SEM measurement value) of the silicon coating thin film of Example 1 was 49.6 μm. The thickness value described in the SEM image of Fig. 4 is an example of the thickness measurement result for a portion.

[0064] Additionally, as a result of observing the surface through SEM images (Fig. 4) and EDS images (Figs. 5 and 6), it was found that a uniform coating film was formed without any protruding parts.

[0065]

[0066] Although the embodiments of the present specification have been described in more detail with reference to the attached drawings, the present specification is not necessarily limited to these embodiments, and various modifications may be implemented without departing from the technical spirit of the present specification. Therefore, the embodiments disclosed in this specification are not intended to limit the technical spirit of the present specification, but to explain, and the scope of the technical spirit of the present specification is not limited by these embodiments. Therefore, it should be understood that the embodiments described above are illustrative in all respects and not restrictive. The scope of protection of this specification should be interpreted by the claims, and all technical ideas within a scope equivalent thereto should be interpreted as being included in the scope of rights of this specification.

Claims

1. D 50 This is 30~90㎛ and has a purity of 99.99% or more. Silicone powder for warriors.

2. In paragraph 1, The total metal impurity content is less than 1,000 ppm, Silicone powder for warriors.

3. Step of supplying raw silicon powder to a grinding device; A step of dry grinding the raw material silicon powder in the grinding device; The above crushed silicon powder is passed through a sieve to D 50 A step of selecting silicon powder satisfying 30 to 90 ㎛; and A step of obtaining a silicon powder for use as a solder; comprising: Method for manufacturing silicon powder for use as a solder.

4. In paragraph 3, The above silicon powder for the warrior has a purity of 99.99% or more. Method for manufacturing silicon powder for use as a solder.

5. In paragraph 4, The above silicon powder for soldering has a total metal impurity content of 1,000 ppm or less. Method for manufacturing silicon powder for use as a solder.

6. In paragraph 3, The above raw material silicon powder has a total metal impurity content of 500 ppm or less, and D 50 This 50 to 200 ㎛, Method for manufacturing silicon powder for use as a solder.

7. In paragraph 3, The above grinding device is any one of a roll mill device, a ball mill device, a jet mill device, and a combination thereof. Method for manufacturing silicon powder for use as a solder.

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