KR101554699B1 - Running preparing using quartz - Google Patents

Abstract

The present invention relates to a method of manufacturing a bath using quartz, and more particularly, to a method of manufacturing a bath using quartz, comprising: a washing step (S110) of washing quartz product or quartz after use; A crushing and crushing step (S120) of crushing the washed quartz to crush and crush the crushed quartz to have various particle sizes; A stirring step (S130) of mixing and crushing the crushed and ground particles of different sizes at a predetermined mixing ratio in the crushing and crushing step (S120), and mixing and stirring the crushed and ground particles with water; A forming step (S140) of forming and drying the agitated quartz using a mold or a molding die for producing a bath drawing; A firing step (S150) of firing the formed quartz; And a surface vitrification step (S160) for densifying the tissue with respect to the baked hot water.

Description

[0001] The present invention relates to a quartz-

More particularly, the present invention relates to a method of manufacturing a blanket using quartz, and more particularly, to a method of manufacturing a blanket using quartz, The present invention relates to a manufacturing method for producing a hot water bath using recycled quartz.

In general, the casting process forms a mold, injects the molten metal into the mold, dismantles the mold after the molten metal solidifies, and finishes the process through finishing work. At this time, the molding material, which is the material for forming the mold, is recycled mostly by installing a regenerating device in terms of environment or cost. Generally, a conduit is used as a duct for manufacturing the mold.

These tundo are basically caused by the erosion of the hot water as the molten steel flows, and the material generated in the tundish remains as a cause of the failure of the steel ingot, so that the erosion resistance against the molten steel and the temperature of the molten steel when the molten steel is injected may be lowered over the injection time. It is necessary to prevent the phenomenon of adhesion due to the reaction between the molten steel and the hot water while solidifying the molten steel after the injection of the molten steel.

On the other hand, quartz is a material that is highly used in semiconductor equipment parts, solar photovoltaics, optics, and medical applications because it has high purity (over 99%) and is resistant to high temperatures and stable to chemicals. In addition, a hot water bath can be produced by using this.

Recently, most of the above-mentioned fields have been used as crucibles or equipment parts in the field of photovoltaic and semiconductor manufacturing. Since products made of quartz are mostly disposed of as waste after the end of their life, quartz regeneration methods for recycling quartz have been demanded.

As a conventional quartz regeneration technology, Korean Patent No. 2011-0013242 (Feb., 2011), a method of regenerating a quartz glass member is known. This means that the quartz glass member, which is used in the semiconductor manufacturing process and consumed and deteriorated, is cleaned and regenerated by a method of suppressing the damage of the base material.

Also, Korean Patent No. 2001-0070123 (July 25, 2001) 'Quartz Crucible Recycling Method' is known as a conventional quartz regeneration technique. This is a method in which the inner surface of the quartz crucible after being used for producing the single crystal silicon is subjected to a restoration treatment by one of chemical etching treatment, mechanical polishing treatment and high temperature heat treatment.

However, the above-described conventional quartz regeneration technique is to regenerate by retaining the shape of the quartz member, filling the glass through a heat treatment or a high-temperature heat treatment, etc., There is a limited field to be used for the regeneration, and since it is necessary to perform cleaning and polishing in the state of maintaining the original member shape, workability is deteriorated and the regeneration process for maintaining high purity is difficult.

In addition, in the case of producing a bath by using quartz, it is desired to develop a bath which has a considerable deterioration in the crack of the bath itself and a dense structure.

In order to solve the above problems, an object of the present invention is to provide a manufacturing process of recovering a quartz product that has been discarded in a solar photovoltaic device, a semiconductor equipment component, and the like, and manufacturing a bathtub through processes such as cleaning, crushing, stirring, molding, There is.

Another object of the present invention is to provide a method of manufacturing a hot-water bath which is remarkably deteriorated in the cracking of the hot-water bath itself and is dense in structure when the hot-water bath is produced using quartz.

In order to achieve the above object, the present invention provides a cleaning method comprising: a cleaning step of cleaning a quartz product or quartz after use; Crushing and crushing the crushed quartz to crush and crush the crushed quartz so as to have various particle sizes; Mixing and stirring the crushed and pulverized particles of different sizes in the crushing and pulverizing step at a predetermined mixing ratio, mixing with water and stirring; A molding step of molding and drying the stirred quartz using a mold or a molding die for producing a bath; A calcining step of calcining the formed quartz; And a surface vitrification step (S160) for densifying the tissue with respect to the baked hot water.

In the cleaning step (S110), the foreign substances other than quartz protruding from the quartz are removed by a physical removal method, the foreign substances adhered to the surface are etched by using chemicals, and the pH of the water is adjusted to pH 6.0 to 8.0 , Followed by rinsing and exhaust drying, followed by cleaning. The present invention also provides a method of manufacturing a bathtub using quartz.

Also, in the crushing and crushing step (S120), crushing is carried out with a crushing crusher having a size of 200mesh or less so that the particle diameter is several millimeters and crushed to a particle size of several to several tens of 탆 with a milling crusher having a size of 2000mesh or less The present invention also provides a method for manufacturing a bath using quartz.

In addition, the present invention provides a method for manufacturing a hot-water bath using quartz, characterized in that it is produced in the form of a slurry finely pulverized using a ball mill in the crushing and crushing step (S120).

In addition, in the stirring step (S130) of the present invention, the crushed and ground raw materials are sorted by particle size, the selected particles are mixed at a predetermined ratio, and water is added to the mixed particles and stirred. The present invention also provides a manufacturing method.

In the present invention, the size of the quartz particles agitated in the stirring step (S130) is in the range of 0.003 mm to 0.035 mm particles 25-40 wt%, 0.035 mm to 0.045 mm particles 15-30 wt%, 0.045 mm- Wherein the mixture is stirred in an amount of 1 to 30 wt%, 0.145 to 0.3 mm, 1 to 30 wt%, and 0.3 to 1.5 mm, and 10 to 40 wt%, respectively.

In the stirring step (S130), quartz, water, a feldspar raw material and a dispersing agent are mixed and agitated in the stirring step (S130), wherein 45 to 90% by weight of quartz, 7 to 50% by weight of water, 0 to 5% by weight of feldspar raw materials, 0 to 3% by weight based on the total weight of the quartz crucible.

Further, in the present invention, the calcining step (S150) is a calcining step in which the preheating step, the high-temperature calcination step, and the cooling step are sequentially performed, and the high-temperature calcination is performed at a high temperature of 1100 to 1400 ° C. to provide.

Further, the present invention provides a method of manufacturing a hot-water bath using quartz, characterized in that the surface is vitrified by applying a high temperature of 1500 to 3000 ° C in the surface vitrification step (S160).

The present invention has the effect of reducing the waste of resources and manufacturing cost by improving the purity of the quartz which is the waste of the quartz product and recycling it.

In addition, in the method of manufacturing the hot-rolled wastewater using quartz according to the present invention, the regenerated quartz product is recovered again, washed, crushed, pulverized, stirred, molded and fired to repeat the regeneration in such a range that the contamination is not increased in the quartz product It can be recycled.

In addition, the method of manufacturing a bath with quartz according to the present invention significantly reduces the cracks in the bath, and has a compact structure.

1 is a view illustrating a process of manufacturing a bathtub using quartz according to an embodiment of the present invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described in detail with reference to the accompanying drawings. First, it should be noted that, in the drawings, the same components or parts have the same reference numerals as much as possible. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted so as to avoid obscuring the subject matter of the present invention.

The terms " about ", " substantially ", etc. used to the extent that they are used herein are intended to be taken to mean an approximation of, or approximation to, the numerical values of manufacturing and material tolerances inherent in the meanings mentioned, Accurate or absolute numbers are used to help prevent unauthorized exploitation by unauthorized intruders of the referenced disclosure.

The present invention is characterized by manufacturing a bathtub using quartz, wherein the bathtub manufacturing method according to the present invention comprises: a washing step of washing the quartz product or quartz after use; Crushing and crushing the crushed quartz to crush and crush the crushed quartz so as to have various particle sizes; Mixing and stirring the crushed and pulverized particles of different sizes in the crushing and pulverizing step at a predetermined mixing ratio, mixing with water and stirring; A molding step of molding and drying the stirred quartz using a mold or a molding die for producing a bath; A calcining step of calcining the formed quartz; And a surface vitrification step for densifying the tissue against the baked hot water.

1 is a view illustrating a process of manufacturing a bathtub using quartz according to an embodiment of the present invention.

The present invention can be applied to a quartz process in which a quartz used as another product is recycled and used or a new quartz is used to perform a cleaning step 110, a crushing and grinding step S120, a stirring step S130, a forming step S140, And the surface vitrification step (S160), and further the inspection step (S170) may be performed.

In the present invention, the cleaning step (S110) removes foreign matter in order to increase the purity of the quartz so that the foreign matter can be removed by a physical or chemical method. More specifically, foreign matter other than quartz adhered to quartz is removed by a physical removal method, followed by etching using a chemical agent, rinsing, drying and cleaning.

The physical cleaning method is a method of removing foreign substances using a cutter and a polishing machine. The chemical cleaning method is a method of cleaning after rinsing and rinsing and exhaust drying so as to have a pH of 6.0 to 8.0 after etching with a chemical agent. The cleaning step may be performed by either a physical cleaning method or a chemical cleaning method, or both of them may be cleaned by a mixed treatment.

The quartz products are used in various fields such as solar light, semiconductor, optical instruments, and medical applications. In the description of the present invention, the reproduction of quartz used in the field of solar light and semiconductor will be described.

The quartz products used as solar crucibles have polysilicon attached to quartz. Quartz used in the photovoltaic field is used to make crucibles for manufacturing ingots made of polysilicon, and the quartz is in a state where the polysilicon is attached. To obtain high-purity quartz, the polysilicon must be removed from the quartz. First, the polysilicon is removed from the quartz by a physical method.

Because polysilicon is molten in a quartz crucible, the adhesion between polysilicon and quartz is so strong that it removes the polysilicon from the quartz with sharp metal (eg, using a diamond cutter) and a hammer. The following can be removed by a chemical method: etching the polysilicon attached to the quartz is chosen. The remaining polysilicon deposited on the quartz is etched by the chemical, which may be the polysilicon etch chemistry commonly used in semiconductor processes.

When etching with a chemical agent is performed, the substrate is contaminated with an etching agent, so that the substrate is cleaned and rinsed. Rinse treatment is carried out using a rinse solution and water until the pH of the water becomes pH 6.0 to 8.0 in the rinse treatment.

After the rinsing treatment, forced drying is performed in an exhaust state at a high temperature of 100 DEG C or more to prevent contamination by moisture.

Secondly, quartz products used as semiconductor equipment components in the semiconductor field are used in various processes, so foreign substances may be adhered on quartz and contaminated. Since quartz products used in semiconductor equipment components are thinner than solar photovoltaics, only the chemical etching method can be used without physical removal. Chemicals for the removal of contaminated contaminants from quartz products used in semiconductor equipment components are HF: HNO ₃ ; H ₂ O can be used in a weight ratio of 1: 3: 4 to 1: 5: 8 (where H ₂ O is DI water) at a temperature of 10 to 30 ° C. until the foreign substances on the surface are completely removed.

Similarly, the cleaning step (S110) can be completed by rinsing with a rinse solution and water until the pH of the water becomes pH 6.0 to 8.0 in the rinse treatment after the etching treatment.

After the cleaning step S110, there is a crushing and crushing step (S120) of processing the bulk quartz material to have a desired particle size, distribution and shape.

In order to use the quartz material or to use new quartz as the material of the bath, it is necessary to crush or crush the quartz to a certain size or less. The crushing and crushing process is indispensable for crushing the quartz material to a certain size and dissolving it or for producing slurry casting material in powder form.

The crushing and crushing step is a crushing crusher having a size of not more than 200 mesh and crushed to a particle size of 1 to 10 mm and a particle size of several to several tens of 탆 (e.g., 1 to 99 탆) And crushing.

The crushing step may be first crushed to a size of several centimeters, and further crushed to a size of several millimeters by secondary crushing. Crushing is a process of lowering the particle size to a few mm (eg, 1 to 10 mm) of a material having a predetermined size or larger. Generally, a jaw crusher, a cone crusher, or an impact crusher is generally used. In the case of dissolving quartz, a product made by a crushing process is suitable.

The pulverizing step is a step of pulverizing the granulated particles made by the pulverization into a powder form so as to have a size of several to several tens of 탆 (e.g., 1 to 99 탆). In case of ceramic material, it is applied in powder form or used as sintering material. Ball Mill, Attrition Mill, Vibratory Mill and Roll Mill can be used to make crushed raw materials into powder form.

In addition, it may be pulverized in a wet state in the pulverization step. In this case, the pulverized slurry may be prepared using a ball mill.

After the crushing and crushing step (S120), the stirring step (S130) is performed. In the stirring step (S130), the crushed and ground quartz material is sorted by particle size, and the quartz raw material is mixed with the selected particles at a predetermined ratio , And water is added to the mixed quartz raw material and stirred.

As an example, in order to select crushed and ground raw materials, crushed and pulverized quartz are selected using a separator, and these are mixed at a proper ratio.

At the time of stirring, different particle sizes are mixed at an appropriate ratio, and the mixed raw materials are mixed with water at a weight ratio of 7 to 50% by weight and stirred. The stirring time is continued until the contents are sufficiently stirred. At this time, the stirring proceeds in a vacuum state and the degree of vacuum is performed in a stirring step (S130) using a vacuum stirrer of 10E (-2 to -5) torr.

The stirring ratio of the quartz particles according to the size of the agitated quartz particles is as follows.

25 to 40 wt% of particles of 0.003 mm to 0.035 mm (0.003 mm or more and less than 0.035 mm), 15 to 30 wt% of particles of 0.035 mm to 0.045 mm, 15 to 30 wt% of particles of 0.045 mm to 0.145 mm, 1 to 30% by weight and 0.3 to 1.5 mm particles 10 to 40% by weight.

When the agitated quartz particles are mixed and agitated at the above ratios, cracks are not generated when firing is performed thereafter.

Further, a small amount of dispersant can be added to prevent the separation of the particle size, and a small amount of the feldspar raw material can be mixed to lower the sintering temperature. That is, quartz, water, a feldspar raw material and a dispersing agent can be mixed and agitated, and it is possible to mix the quartz, the water, the feldspar raw material and the dispersing agent in an amount of 45 to 90 wt%, quartz 7 to 50 wt%, feldspar raw material 0 to 5 wt% Mixing is possible.

After the stirring is completed, a molding step (S140) is performed in which the thin molding material filled with the stirring material is filled in the molding die and molded.

Gypsum or the like to produce a gypsum mold and then charge the stirred material. At this time, a method of pressure injection molding or general injection molding is used.

When the molding is performed for a certain time in the mold for manufacturing the mold, the molded product is separated from the mold. Dehydration too soon will cause too much moisture and breakage. If it is molded for too long, there is a high possibility of cracking. At the time of desorption, the water content of the product is preferably about 5 to 20%. When demoulding is complete, transfer to dry room and dry. Drying is likely to be delayed or cracked if it is carried out at low or high temperatures.

It is preferable that the molding step is performed in a molding die at a water content in the range of 5 to 20%, and the demolded molded article is dried at room temperature to 200 ° C.

After the forming step S140, the firing step S150 is performed. The sintering step (S150) is performed by performing the preheating step, the high-temperature sintering step and the cooling step in sequence, the preheating and cooling are performed at about 100 ° C / min, and the high temperature sintering is performed at a high temperature of 1100 to 1400 ° C Preferably, firing is carried out for about 18 to 22 hours.

The firing step (S150) is performed by using a kiln or a tunnel furnace.

When the firing step S150 is completed, the surface vitrification step S160 for making the surface of the surface finer is performed.

After the baking, the surface roughness (toughness) is large and the bonding force between the tissues is small, so that it is easily broken. Since the molten metal has a high specific gravity and a high temperature, it has to have high bonding strength. Particularly, a product having a small foreign substance should have a good structure force on the surface contacting with the molten metal.

In addition, quartz is chemically very stable, but it may require physical diffusion or chemical reaction with substances that are susceptible to reaction at high temperatures. To prevent this, quartz surfaces must be subjected to a surface treatment capable of withstanding high temperatures. At this time, the surface treatment substance should have a dense structure and chemically, the reaction should not occur with the substance inside the bath.

The surface vitrification step (S160) is to prevent corrosion and infiltration due to adsorption and reaction of molten metal in the molten metal. For this purpose, by applying a high temperature (1500 to 3000 ° C) using an arc generator or the like, (Glass), the surface texture becomes dense and the surface roughness can be reduced.

Therefore, the surface vitrification step (S160) allows the internal structure of the bath to be dense and the surface roughness to be small, thereby minimizing the possibility of foreign matter generation.

After the surface vitrification step (S160), an inspection step (S170) for inspecting the produced hot water may be additionally performed.

As a result of the test, it is preferable that the bath temperature using the quartz produced has a compressive strength of 400 kg / cm 2 or more, a specific gravity of about 1.9, and a porosity of 6 to 12%.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the inventions. It will be clear to those who have knowledge of.

Claims (9)

A cleaning step (S110) of cleaning the spent quartz product or quartz after use;
A crushing and crushing step (S120) of crushing the washed quartz to crush and crush the crushed quartz to have various particle sizes;
A stirring step (S130) of mixing and crushing the crushed and ground particles of different sizes at a predetermined mixing ratio in the crushing and crushing step (S120), and mixing and stirring the crushed and ground particles with water;
A forming step (S140) of forming and drying the agitated quartz using a mold or a molding die for producing a bath drawing;
A firing step (S150) of firing the formed quartz; And
And a surface vitrification step (S160) for densifying the tissue with respect to the baked hot water,
The cleaning step S110 removes foreign materials other than quartz protruding from the quartz by a physical removal method, etches the foreign substances adhered to the surface with chemicals, rinses the solution so that the pH of the water becomes pH 6.0 to 8.0 Followed by exhaust drying after rinsing to clean,
The size of the quartz particles agitated in the stirring step (S130) is 25 to 40% by weight, 0.005 to 20% 0.1 to 0.3 mm particles of 1 to 30% by weight and 0.3 to 1.5 mm of particles of 10 to 40% by weight,
In the surface vitrification step (S160), the surface texture is dense and the surface roughness is reduced by applying a high temperature of 1500 to 3000 占 폚 in order to prevent corrosion and infiltration due to adsorption and reaction of molten metal in the molten metal. Manufacturing method using hot water.
delete The method according to claim 1,
The crushing and crushing step (S120) is carried out by crushing the crushed material to a size of several millimeters with a coarsely crushing crusher having a size of 200 mesh or less, and pulverizing the crushed material to a particle size of several to several tens of micrometers with a milling crusher of 2,000 mesh or less A method for manufacturing a bath using quartz.
The method according to claim 1,
Wherein the slurry is pulverized in a pulverizing and grinding step (S120) using a ball mill.
The method according to claim 1,
Wherein the stirring step (S130) comprises selecting the crushed and ground raw materials by particle size, mixing the selected particles at a predetermined ratio, and adding water to the mixed particles and stirring the mixture.
delete The method according to claim 1,
Wherein the mixture is stirred while mixing the quartz, water, feldspar raw material and dispersant in the stirring step (S130), wherein the quartz, water, feldspar raw material and dispersant are mixed and stirred. By weight based on the total weight of the quartz.
The method according to claim 1,
Wherein the firing step (S150) is performed by sequentially performing a preheating step, a high-temperature firing step and a cooling step, and the high-temperature firing is performed at a high temperature of 1100 to 1400 ° C.
delete

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