KR101739727B1 - - - functional graphite crucible for promoting gas-solid reactions system to produce synthetic powder with gas solid reactions - Google Patents

Abstract

The present invention relates to a graphite crucible for promoting a gas-solid reaction, and more particularly to a graphite crucible for promoting a gas-solid reaction, which comprises a bottom surface having a machining hole formed thereon and a side surface protruded from a bottom surface, A system for producing a powdered composite through a gas-solid reaction and a functional graphite crucible for gas-solid reaction promotion, wherein the reaction gas flows into the crucible.

Description

[TECHNICAL FIELD] The present invention relates to a graphite crucible for promoting a gas-solid reaction and a system for producing a powder composite through a gas-solid reaction,

The present invention relates to a system for producing a powdered composite through a functional graphite crucible for gas-solid reaction promotion and a gas-solid reaction, and more particularly to a system for producing a powdery composite through a gas- Functional graphite crucible for gas-solid reaction promotion and a system for producing a powdery composite through a gas-solid reaction.

To expose the solid powder to the reaction gas and mass-produce the powder synthesis product, the crucible containing the solid powder in the box-type high-temperature reaction furnace is laminated, the internal temperature is raised up to a predetermined value by the high-temperature reaction, The reaction gas is injected into the reaction furnace. At this time, holes are formed on the upper side of the crucible to communicate the inside of the reaction furnace and the inside of the crucible.

The solid powder contained in the crucible is in close contact with the bottom surface of the crucible. On the surface of the solid powder, the reaction occurs immediately after the reaction gas is introduced into the crucible. On the other hand, in the solid powder, the reaction gas penetrates through the pores of the solid powder, Lt; / RTI >

That is, in order for the reactive gas to reach the solid powder adhering to the bottom of the crucible, the penetration diffusion time of the reactive gas is required.

Thus, in order to obtain a completely powdered composite, the reaction time calculated based on the penetration diffusion rate had to be sufficiently elapsed.

Korean Registered Patent No. 10-1390799 (Apr. 24, 2014)

An object of the present invention is to provide a functional graphite crucible for facilitating gas-solid reaction, which increases a contact area between a solid powder and a reactive gas so as to shorten the penetration diffusion time of the reactive gas.

Another object of the present invention is to provide a system for producing a powdery composite through a gas-solid reaction, which can produce a large amount of powdery product in a shorter time than in the prior art by shortening the penetration diffusion time of the reactive gas .

In order to accomplish the above object, the present invention provides a graphite crucible for promoting a gas-solid reaction, the graphite crucible including a bottom surface having a processing hole formed thereon and a side surface protruding from the bottom surface to form a predetermined space.

Further, it may include a graphite filter film adhered to one surface of the bottom surface so as to cover the processing hole.

Also, the graphite filter lid can be mounted on the side so as to cover the space.

In addition, a plurality of seating projections may be formed at equal intervals on the upper side of the side surface.

In addition, a plurality of seating grooves into which the end portions of the seating projections are inserted may be formed on the bottom surface, and the depth of the seating grooves may be smaller than the length of the seating projections.

Further, the cross section of the processing hole may be trapezoidal or stepped.

In order to accomplish the above object, the present invention provides a system for producing a powdery composite through a gas-solid reaction, comprising: a plurality of graphite crucibles containing solid powder in a box-type high-temperature reactor; Wherein the reaction gas flows into the graphite crucible at the same time from the upper side and the lower side of the graphite crucible, in the system for mass production of the powdery synthesis product by injecting the reaction gas into the graphite crucible.

Further, the graphite crucible may include a bottom surface formed with a machining hole, and a side surface protruded from the bottom surface to form a predetermined space with the bottom surface.

Further, a graphite filter film may be adhered to one surface of the bottom surface to cover the machining holes, and a plurality of seating protrusions may be formed at equal intervals on the side surface.

Further, the reaction gas enters the upper side of one of the plurality of graphite crucibles through the seating projections, and the reaction gas can enter the lower side of the other graphite crucible through the processing hole positioned above the seating projections.

Specific details of other embodiments are included in the " Detailed Description of the Invention "and the accompanying drawings.

BRIEF DESCRIPTION OF THE DRAWINGS The advantages and / or features of the present invention and the manner of achieving them will be apparent by reference to various embodiments described in detail below with reference to the accompanying drawings.

However, the present invention is not limited to the configurations of the embodiments described below, but may be embodied in various other forms, and each embodiment disclosed in this specification is intended to be illustrative only, It will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

According to the present invention, the reactive gas flows in the upper and lower directions of the graphite crucible, respectively, whereby the penetration and diffusion speed of the reactive gas through the pores of the solid powder is drastically shortened compared with the conventional case, The powder synthesis product production time can be shortened.

This is explained in more detail as follows. The reaction gas flows into the graphite crucible simultaneously at the lower side and the upper side of the graphite crucible.

As a result, the upper and lower surfaces of the solid powder contained in the graphite crucible are brought into contact with the reactive gas at the same time, and penetration diffusion of the reactive gas occurs on both surfaces. Thus, the reaction time between the solid powder and the reaction gas is shortened.

Particularly, since the reaction time is shortened, the productivity of the powder synthetic product is increased. In addition, the uniformity of the reaction product, that is, the powder synthesis product, is improved.

1 is a perspective view of a functional graphite crucible for promoting gas-solid reaction in an embodiment of the present invention,
FIG. 2 is a plan view and a side view of a functional graphite crucible for promoting gas-solid reaction shown in FIG. 1;
FIG. 3 is a perspective view of a state in which a plurality of functional graphite crucibles for promoting gas-solid reaction shown in FIG. 1 are stacked,
Fig. 4 is a cross-sectional view of a plurality of stacked graphite crucibles of Fig. 3,
5 is an illustration of a system for producing a powdered composite through a gas-solid reaction of an embodiment of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

Before describing the present invention in detail, terms and words used herein should not be construed as being unconditionally limited in a conventional or dictionary sense, and the inventor of the present invention should not be interpreted in the best way It is to be understood that the concepts of various terms can be properly defined and used, and further, these terms and words should be interpreted in terms of meaning and concept consistent with the technical idea of the present invention.

That is, the terms used herein are used only to describe preferred embodiments of the present invention, and are not intended to specifically limit the contents of the present invention, It should be noted that this is a defined term.

Furthermore, in this specification, the singular forms "a", "an", and "the" include plural referents unless the context clearly dictates otherwise, and it should be understood that they may include singular do.

Where an element is referred to as "comprising" another element throughout this specification, the term " comprises " does not exclude any other element, It can mean that you can do it.

Further, when it is stated that an element is "inside or connected to" another element, the element may be directly connected to or in contact with the other element, A third component or means for fixing or connecting the component to another component may be present when the component is spaced apart from the first component by a predetermined distance, It should be noted that the description of the components or means of 3 may be omitted.

On the other hand, it should be understood that there is no third component or means when an element is described as being "directly connected" or "directly connected" to another element.

Likewise, other expressions that describe the relationship between the components, such as "between" and "immediately", or "neighboring to" and "directly adjacent to" .

In this specification, terms such as "one side", "other side", "one side", "other side", "first", "second" Is used to clearly distinguish one element from another element, and it should be understood that the meaning of the element is not limited by such term.

It is also to be understood that terms related to positions such as "top", "bottom", "left", "right" in this specification are used to indicate relative positions in the drawing, Unless an absolute position is specified for these positions, it should not be understood that these position-related terms refer to absolute positions.

Moreover, in the specification of the present invention, terms such as " to, "" module, " Or software, or a combination of hardware and software.

In this specification, the same reference numerals are used for the respective components of the drawings to denote the same reference numerals even though they are shown in different drawings, that is, the same reference numerals throughout the specification The symbols indicate the same components.

In the drawings attached to the present specification, the size, position, coupling relationship, and the like of each constituent element of the present invention may be partially or exaggerated or omitted or omitted for the sake of clarity of description of the present invention or for convenience of explanation May be described, and therefore the proportion or scale may not be rigorous.

Further, in the following description of the present invention, a detailed description of a configuration that is considered to be unnecessarily blurring the gist of the present invention, for example, a known technology including the prior art may be omitted.

1 to 4, a graphite crucible for graphitizing solid-gas reaction (C) according to an embodiment of the present invention includes a bottom surface 100 having a processing hole 110 formed thereon, a bottom surface 100, And a side surface 200 protruding from the bottom surface 100 to form a predetermined space.

Particularly, the graphite filter film 300 is adhered to one surface of the bottom surface 100 so as to cover the processing hole 110.

The graphite filter film 300 prevents the solid powder from leaking from the crucible through the processing hole 110. Since the graphite filter film 300 has fine holes, the flow of the reactive gas A is smoothly generated.

The diameter of the processing hole 110 is preferably smaller than the diameter or the width of the bottom surface 100, and the number and size thereof can be variously selected as needed. When the bottom surface 100 is circular, the machining hole 110 may be formed to have a diameter slightly smaller than the diameter of the bottom surface 100.

The machining hole 110 is formed so as to have a trapezoidal shape or a stepped shape so as to have a shape which is expanded toward the upper side. Accordingly, the reactive gas A introduced into the bottom of the crucible through the processing hole 110 can contact with the solid powder in a larger area.

The graphite filter lid 400 is mounted on the side surface 200 so as to cover the space formed by the bottom surface 100 and the side surface 200. [ The graphite filter lid 400 prevents foreign matter of a size that can be visually recognized from entering the crucible.

A plurality of seating protrusions 210 are formed on the upper surface of the side surface 200 at regular intervals and a plurality of seating grooves 120 are formed in the bottom surface 100 to receive the ends of the seating protrusions 210. The seating groove 120 is made so that its depth is smaller than the length of the seating projection 210. [

When the plurality of graphite crucibles C are stacked, the seating protrusions 210 are inserted into the seating grooves 120, whereby the graphite crucible C is securely stacked.

When the internal pressure of the reaction furnace 500 is increased by injecting the reactive gas A into the reaction furnace 500, the reaction gas is introduced into the reaction furnace 500 through the gap formed between the mounting protrusions 210 and the mounting protrusions 210 A) flows into the upper portion of the crucible.

The air inside the reaction furnace 500 flowing into the upper portion of the crucible diffuses and is separated and transferred to the upper and lower portions. That is, the air in the reaction furnace 500 flowing into the crucible flows into the surface of the solid powder contained in the crucible and flows into the processing hole 110 of the bottom surface 100 positioned above the solid powder, To contact the bottom surface of the solid powder in contact with the bottom surface 100.

That is, the upper and lower surfaces of the solid powder come into contact with the reactive gas A at the same time. As a result, the reaction gas (A) penetrates and diffuses into the solid powder voids more easily than in the prior art.

A system for producing a powdery composite utilizing the graphite crucible (C) for accelerating gas-solid reaction of an embodiment of the present invention constructed as above is illustrated in Fig.

As shown in FIG. 5, a system for producing a powdery composite through a gas-solid reaction according to an embodiment of the present invention includes a box-shaped reactor 500 and a plurality of stacked gases A heating device 600 for raising the internal temperature of the reaction furnace 500 and an injection device 700 for injecting the reactive gas A into the reaction furnace 500. The graphite crucible C for accelerating the solid reaction, And a relief valve 800 for maintaining the internal pressure of the reactor 500 at a predetermined value or less.

The system for producing the powdery composite through the gas-solid reaction of the embodiment of the present invention as described above is characterized in that the graphite crucible (C) for promoting the gas-solid reaction is provided so that the reaction gas (A) And simultaneously flows into the graphite crucible C from above and below.

As described above, when the internal pressure of the reaction furnace 500 rises in accordance with the injection of the reactive gas A, the reactive gas A is introduced into the space between any one of the plurality of graphite crucibles C And enters the upper side of the graphite crucible C. [

The reaction gas A is moved to the upper surface of the solid powder contained in the graphite crucible C and enters the lower side of the other graphite crucible C through the processing hole 110 positioned above the seating projections 210 .

The reaction gas entering the lower side of the other graphite crucible C through the processing hole 110 comes into contact with the lower surface of the solid powder.

That is, since the upper surface and the lower surface of the solid powder come into contact with the reactive gas A at the same time, the contact area between the solid powder and the reactive gas A increases.

Experiments were conducted to produce aluminum nitride according to the following formula (1) utilizing the above-described functional graphite crucible (C) for gas-solid reaction promotion of the present invention and a system for producing a powder synthesis product through a gas- .

The internal temperature of the reactor 500 was raised to 1,700 degrees Celsius and the internal pressure was adjusted to a vacuum of 0.2 Torr. A mixture of powders of alumina (Al2O3) and graphite powder at a molar ratio of 1: 3.2 was reacted with nitrogen (N2) gas to produce aluminum nitride (AlN).

The above generation experiment will be described in more detail as follows. 1 kg of mixed powder sample was charged into the functional graphite crucible (C) for promoting gas-solid reaction of the present invention, and five graphite crucibles (C) were stacked in the reactor 500.

The internal temperature of the reaction furnace 500 was raised to 1,700 degrees Celsius according to the automatic temperature control program provided in the reaction furnace 500 while the internal pressure of the reaction furnace 500 was lowered. Then, nitrogen gas was injected into the reactor 500 at a rate of 40 liters per minute to generate a reaction represented by the above formula (1).

After completion of the reaction, samples for analysis reaction products were collected for each graphite crucible (C). X-ray diffraction analysis of the sample confirmed that the main component was aluminum nitride (AlN).

Then, the carbon (C) and oxygen (O) components remaining in the reaction product for each graphite crucible (C) were analyzed using a gas analyzer to measure the residual carbon concentration.

Also, the progress of the reaction was judged from the carbon and oxygen analysis results, and the homogeneity of the reaction product in the case where the processing hole 110 was formed on the floor 100 of the graphite crucible (C) .

In order to do this, a graphite crucible C in which a machining hole 110 is not formed and a graphite crucible in which 25 machining holes 110 having a diameter of 20 millimeters are formed concentrically from the center And a graphite crucible (C) in which 43 machining holes (110) having a diameter of 10 millimeters were formed concentrically from the center on the bottom surface (100) were subjected to the same reaction experiment Lt; / RTI >

Then, a certain amount of sample was sampled for each graphite crucible (C), and residual carbon and oxygen were analyzed. The upper graphite crucible (C), and the lower graphite crucible (C) in the order of 1, 2, 3, 4, and 5. The results are summarized in Table 1 below.

Stacking sequence \ Crucible type A B C C, wt% O, wt% C, wt% O, wt% C, wt% O, wt% One 5.89 0.64 3.49 0.46 3.72 0.55 2 6.25 0.75 3.52 0.52 3.56 0.47 3 7.14 0.73 3.78 0.62 3.85 0.74 4 6.82 0.82 3.67 0.55 3.74 0.62 5 7.95 0.89 3.56 0.78 3.95 0.68

As shown in Table 1, in the case of the graphite crucible C in the form of B and C, in which the machining hole 110 is formed on the bottom surface 100 of the graphite crucible C, the machining hole 110 is formed It is understood that the amount of carbon and oxygen remaining in the sample is smaller than that of the graphite crucible (C) of the A-type which is not used.

Further, in each case, the amount of carbon and oxygen remaining in the graphite crucible (C) in the uppermost layer was smaller than that in the graphite crucible (C) in the bottom layer.

In the case of the graphite crucible A in the form of B, the amount of residual carbon is 5.49 to 7.95% and the amount of residual oxygen is 0.64 to 0.89%, while in the case of the graphite crucible B in the form B, %, Residual oxygen content of 0.46 ~ 0.78%, and residual carbon content of 3.56 ~ 3.95% and residual oxygen content of 0.47 ~ 0.74% for C type graphite crucible (C).

The amount of residual carbon is smaller in the case of the B and C type graphite crucible C in which the machining hole 110 is formed than in the case of the A type graphite crucible C in which the machining hole 110 is not formed, (C), the gas-solid reaction occurs more rapidly and the homogeneity of the reaction product can be judged to be higher than when the graphite crucible (C) is used.

As described above, when the functional graphite crucible (C) for promoting a gas-solid reaction of the present invention and the system for producing a powder synthesis product through a gas-solid reaction are used, the graphite crucible (C) The reaction gas (A) is introduced into the reaction vessel (A), whereby the penetration and diffusion rate of the reaction gas (A) through the pores of the solid powder is drastically shortened compared with the conventional art, and ultimately the powder synthesis product production time can be shortened.

This is explained in more detail as follows. The reaction gas A flows into the graphite crucible C at the lower and upper sides of the graphite crucible C at the same time.

As a result, the upper and lower surfaces of the solid powder contained in the graphite crucible (C) come into contact with the reactive gas (A) at the same time, and penetration diffusion of the reactive gas (A) occurs on both surfaces. Therefore, the reaction time between the solid powder and the reactive gas (A) is shortened.

Particularly, since the reaction time is shortened, the productivity of the powder synthetic product is increased. In addition, the uniformity of the reaction product, that is, the powder synthesis product, is improved.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is evident that many alternatives, modifications and variations will be apparent to those skilled in the art. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

In addition, since the present invention can be embodied in various other forms, the present invention is not limited by the above description, and the above description is intended to be a complete description of the present invention, It will be understood by those of ordinary skill in the art that the present invention is only provided to fully inform the person skilled in the art of the scope of the present invention and that the present invention is only defined by the claims of the claims.

100: bottom surface 110: machining hole
120: seat groove 200: side
210: mounting projection 300: graphite filter membrane
400: Graphite filter lid 500: Reactor
600: heating device 700: injection device
800: relief valve C: graphite crucible
A: Reaction gas

Claims (10)

A bottom surface formed with a machining hole;
A side surface protruding from the bottom surface to form a predetermined space with the bottom surface;
And a graphite filter film adhered to the bottom surface to cover the processing hole,
A plurality of processing holes are formed radially with respect to a center of the bottom surface,
And the processing hole is expanded along the height direction so that the reactive gas passing through the processing hole is diffused.
delete delete The method according to claim 1,
And a plurality of seating protrusions are formed at regular intervals on the upper side of the side surface of the graphite crucible for promoting gas-solid reaction.
5. The method of claim 4,
A plurality of seating recesses are formed in the bottom surface, into which the end portions of the seating protrusions are inserted,
Wherein a depth of the seating groove is smaller than a length of the seating projection.
The method according to claim 1,
Wherein a cross-
Trapezoidal or stepped graphite crucible for gas-solid reaction promotion.
There is provided a system for stacking a plurality of graphite crucibles containing solid powder in a box type high temperature reactor, raising the internal temperature of the reactor, and injecting a reaction gas into the reactor to mass-
The reaction gas flows into the graphite crucible at the same time from the upper side and the lower side of the graphite crucible,
In the graphite crucible,
A bottom surface formed with a machining hole;
A side surface protruding from the bottom surface to form a predetermined space with the bottom surface;
And a graphite filter film adhered to the bottom surface to cover the processing hole,
A plurality of processing holes are formed radially with respect to a center of the bottom surface,
Wherein the processing hole is expanded along the height direction so that the reaction gas having passed through the processing hole is diffused, thereby producing a powdery composite through a gas-solid reaction.
delete 8. The method of claim 7,
A system for producing a powdered composite through a gas-solid reaction in which a plurality of seating protrusions are formed at equal intervals on the side surface.
10. The method of claim 9,
The reaction gas enters the upper side of one of the plurality of graphite crucibles through the space between the seating projections,
Wherein the reaction gas enters the bottom of another graphite crucible through a processing hole positioned above the seating projection.

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