CN113842658A - Refining method of liquid ALD precursor - Google Patents
Refining method of liquid ALD precursor Download PDFInfo
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- CN113842658A CN113842658A CN202111117166.8A CN202111117166A CN113842658A CN 113842658 A CN113842658 A CN 113842658A CN 202111117166 A CN202111117166 A CN 202111117166A CN 113842658 A CN113842658 A CN 113842658A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/148—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step in combination with at least one evaporator
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention discloses a refining method of a liquid ALD precursor, which comprises the following steps: rectifying a low-purity crude product of a liquid ALD precursor; pretreating the purifying material polyethylene porous particles, and filling the purifying tower with the pretreated purifying material; and (4) flowing the rectified components into a purification tower filled with purification materials, and carrying out purification treatment at a boiling point temperature to obtain a high-purity product. The refining method is simple to operate and wide in application range, various ALD precursors can be refined, in addition, the polyethylene porous purification particles are high-molecular materials, metal ions cannot be released to pollute the raw materials, impurity ions can be locked, the purity of the ALD precursor compounds purified by the polyethylene porous purification particles is as high as 99.9999%, and the purity requirement of the ALD precursor compounds can be met.
Description
Technical Field
The invention relates to a purification method of a liquid compound, in particular to a refining method of a liquid ALD precursor.
Background
In a Complementary Metal Oxide Semiconductor (CMOS) process, the feature size is typically represented by the width of the "gate," i.e., the channel length of the Metal Oxide Semiconductor (MOS) device. In general, the smaller the feature size, the higher the integration of the chip, the better the performance, and the lower the power consumption. The traditional gate dielectric material is SiO2With the development of the integrated circuit industry, the technology is well developedWith silicon dioxide gate thicknesses approaching 2-3nm, direct electron tunneling and high leakage currents severely hamper device reliability. These problems can be solved by replacing SiO with a high dielectric constant (high-K) material2The solution is to be solved.
The high-K gate dielectric can increase the physical thickness of the gate dielectric while keeping the gate capacitance unchanged, thereby achieving the dual purposes of reducing gate leakage current and improving the reliability of the device, wherein the high-K material of nitride and metal oxide is the most promising to replace SiO2As a gate dielectric material.
A common metal oxide type high-K material is TiO2、ZrO2、HfO2The ALD precursor sources such as tetrakis (dimethylamino) titanium, tetrakis (dimethylamino) hafnium, tetrakis (methylethylamino) titanium, tetrakis (methylethylamino) zirconium, tetrakis (methylethylamino) hafnium, tetrakis (diethylamino) titanium, tetrakis (diethylamino) zirconium, tetrakis (diethylamino) hafnium, etc. to which they correspond are all liquid phases. Because the purity of the precursor is crucial to the performance of the thin film in the atomic layer deposition process, the purity requirement of the precursor in the semiconductor industry is very strict, but the purity of the ALD precursor prepared at present is difficult to reach 99.9999%, and a purification method is urgently needed to improve the purity of the ALD precursor.
Disclosure of Invention
In order to solve the technical problems, the invention provides a refining method of a liquid ALD precursor, which is characterized in that the liquid ALD precursor with low purity is rectified and then purified by a special purification material to obtain a product with the purity of 99.9999%.
The invention provides the following technical scheme:
the invention provides a refining method of a liquid ALD precursor, which comprises the following steps:
rectifying a crude product of the liquid ALD precursor;
pretreating the purification material, and filling the purification tower with the pretreated purification material;
flowing the rectified components into a purification tower filled with purification materials, carrying out purification treatment at a boiling point temperature, and discharging after purification to obtain a high-purity ALD precursor;
the purification material is porous particles, the porous particles are provided with through pore channels with hollow bending structures, and the pore channels are provided with a plurality of U-shaped bends; the boiling point temperature is the boiling point temperature of the liquid ALD precursor in a decompression state, and the boiling point temperature range is 50-120 ℃; the high purity is a purity higher than 99.9999%.
Further, the boiling point temperature is preferably 0.1 mmHg.
Further, the liquid ALD precursor is one of tetrakis (dimethylamino) titanium, tetrakis (dimethylamino) hafnium, tetrakis (methylethylamino) titanium, tetrakis (methylethylamino) zirconium, tetrakis (methylethylamino) hafnium, tetrakis (diethylamino) titanium, tetrakis (diethylamino) zirconium, and tetrakis (diethylamino) hafnium.
Further, the mesh number of the purification material is 100-200.
Further, the purification material is ultra-high molecular weight polyethylene porous particles.
Polyethylene granule with porous structure, its pore structure is similar to the crooked pipeline of cavity, the material flows into the purification tower bottom of the tower through feed valve, bottom heating device heats the material at the bottom of the tower, temperature control is at the boiling temperature of target product, the material is heated and is evaporated, impurity can be taken to the purification layer from the tower bottom by the material, material steam shuttles back and forth in the pore of each purification granule, take place the phase transition in pore U-shaped bend department, form the hydrops, form liquid seal gradually, and impurity metal ion can be locked at the pore bottom, in order to reach the purification effect.
The polyethylene porous material is easy to age and even degrade at high temperature, so that the pressure is reduced in the purification process to reduce the boiling point, on one hand, the polyethylene can be prevented from aging and polluting the purified material, and on the other hand, the service life of the purified material can be prolonged.
Further, the molecular weight of the ultra-high molecular weight polyethylene porous particles is 1500000-3000000.
Because the purified material has certain corrosivity, in the organic high-molecular porous material meeting the purification requirement, the chemical resistance of the polyethylene with the ultrahigh molecular weight is excellent, the secondary pollution of the purified material to a purified product in the purification process can be avoided, the polyethylene is low in price, the polymer with the molecular weight of more than 150W can be easily prepared, and the polyethylene porous material with the high molecular weight is used as the purification material, so that the cost is low and the effect is good.
Further, the ultra-high molecular weight polyethylene porous particles have a molecular weight distribution index of 1.1 to 1.7.
Further, the pore size of the ultra-high molecular weight polyethylene porous particles is 0.5 to 1 μm.
Further, the particle size of the ultra-high molecular weight polyethylene porous particles is 3-5 mm.
The polyethylene porous material is used as a purification material, the pore diameter and the particle size of the polyethylene porous material need to be controlled in a proper interval, if the pore diameter is too large, the flow quantity of the material among pores is increased, impurities are easily brought out in the flow process, the impurities cannot be locked in a liquid seal mode, and if the pore diameter is too small, the pore channel is easily blocked, so that the purification effect is poor; in addition, the particle size cannot be too large, the specific surface area of the porous particles is reduced along with the increase of the particle size, and then the purification efficiency is reduced, but the particle size cannot be too small, and the particle size is too small, so that a liquid seal is formed due to pressure drop to block a filler column, and the purification is stopped, therefore, the particle size and the pore size of the polyethylene porous particles need to be controlled in a proper interval to improve the purification efficiency and effect.
Further, the melting point of the polyethylene porous particles is 200-220 ℃.
Further, the pretreatment of the purification material is specifically: washing the purified material with ultrapure water, and drying the washed purified material to obtain a pretreated purified material; the temperature of the drying treatment is 110-150 ℃, and the time of the drying treatment is 12-36 h.
Further, the purification tower sequentially consists of a heating device, a feeding valve, a tower body and a discharging valve from bottom to top; the tower body is used for containing purification materials, and the heating device is used for heating the materials at the bottom of the tower body; the tower body is provided with a heat insulation layer.
Further, the time of the purification treatment is 3-9 h.
And further, after the purification is finished, leaching the recovered purification material by using an alkane solvent, washing by alkali, washing by acid and washing by ultrapure water, and drying for later use.
By means of the scheme, the invention has the beneficial effects that: the invention uses the polyethylene porous particles as the purification material, locks impurity metal ions in the material evaporation process to achieve the purification effect, and the polyethylene is a high molecular material, so that the polyethylene can not release metal ions to pollute the raw material; the method is simple to operate, no harmful waste liquid is generated, various liquid-phase ALD precursors can be purified, the purity of the processed compounds reaches 99.9999%, the purification materials can be recycled, the purification cost is reduced, and the method has a good application prospect in the aspect of industrial production purification.
Drawings
FIG. 1 is a schematic diagram of a purification column apparatus;
FIG. 2 is a schematic cross-sectional view of a porous polyethylene pellet;
fig. 3 is a schematic diagram of a single cell structure inside the porous polyethylene particle.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The experimental methods used in the following examples are conventional methods unless otherwise specified, and materials, reagents and the like used therein are commercially available without otherwise specified.
Example 1: purification of tetrakis (dimethylamino) titanium
Rectifying low-purity tetra (dimethylamino) titanium, and collecting 50 ℃/0.1mmHg fractions; washing the polyethylene porous particles with ultrapure water, drying at 120 ℃ for 24 hours, and filling the purification tower with the dried polyethylene porous particles, wherein the parameters of the polyethylene porous particles are detailed in table 1; and (2) flowing the fraction collected in the step (1) into a purifying tower filled with purifying materials, keeping the fraction at 50 ℃/0.1mmHg for 6 hours, and discharging to obtain high-purity tetra (dimethylamino) titanium.
The purity of the obtained tetra (dimethylamino) titanium is detected by ICP, and the result shows that the purity of the product tetra (dimethylamino) titanium is as high as 99.9999%.
TABLE 1 values of the various parameters of the porous polyethylene particles
Number of meshes | Molecular weight | Molecular weight distribution index | Pore diameter | Particle size |
100 | 1750000 | 1.3 | 0.5μm | 5mm |
Example 2: purification of tetrakis (methylethylamino) titanium
Rectifying low-purity tetra (methylethylamino) titanium, and collecting a fraction at 78 ℃/0.1 mmHg; washing the polyethylene porous particles with ultrapure water, drying at 120 ℃ for 24 hours, and filling the purification tower with the dried polyethylene porous particles, wherein each parameter of the polyethylene porous particles is detailed in table 2; and (2) flowing the fraction collected in the step (1) into a purifying tower filled with purifying materials, keeping the fraction at 78 ℃/0.1mmHg for 6 hours, and discharging to obtain high-purity tetra (methylethylamino) titanium.
The purity of the obtained tetra (methylethylamino) titanium is detected by ICP, and the result shows that the purity of the product tetra (methylethylamino) titanium is as high as 99.9999%.
TABLE 2 values of the various parameters of the porous polyethylene particles
Number of meshes | Molecular weight | Molecular weight distribution index | Pore diameter | Particle size |
100 | 1980000 | 1.4 | 0.6μm | 5mm |
Example 3: purification of tetrakis (methylethylamino) zirconium
Rectifying low-purity tetra (methylethylamino) zirconium, and collecting a fraction at 81 ℃/0.1 mmHg; washing the polyethylene porous particles with ultrapure water, drying at 120 ℃ for 24 hours, and filling the purification tower with the dried polyethylene porous particles, wherein the parameters of the polyethylene porous particles are detailed in table 3; and (2) flowing the fraction collected in the step (1) into a purifying tower filled with purifying materials, keeping the temperature at 81 ℃/0.1mmHg for 6 hours, and discharging to obtain high-purity tetra (methylethylamino) zirconium.
The purity of the obtained tetrakis (methylethylamino) zirconium is detected by ICP, and the result shows that the purity of the product tetrakis (methylethylamino) zirconium is as high as 99.9999%.
TABLE 3 values of the various parameters of the porous polyethylene particles
Number of meshes | Molecular weight | Molecular weight distribution index | Pore diameter | Particle size |
100 | 2200000 | 1.3 | 0.7μm | 4mm |
Example 4: purification of tetrakis (diethylamino) hafnium
Rectifying low-purity tetra (diethylamino) hafnium, and collecting 130 ℃/0.1mmHg fractions; washing the polyethylene porous particles with ultrapure water, drying at 120 ℃ for 24 hours, and filling the purification tower with the dried polyethylene porous particles, wherein each parameter of the polyethylene porous particles is detailed in table 4; and (2) flowing the fraction collected in the step (1) into a purifying tower filled with purifying materials, keeping the temperature at 130 ℃/0.1mmHg for 6 hours, and discharging to obtain the high-purity tetra (diethylamino) hafnium.
The purity of the obtained tetrakis (diethylamino) hafnium was measured by ICP, and the purity of the product tetrakis (diethylamino) hafnium was as high as 99.9999%.
TABLE 4 values of various parameters of the porous particles of ethylene
Number of meshes | Molecular weight | Molecular weight distribution index | Pore diameter | Particle size |
200 | 2500000 | 1.4 | 0.8μm | 4mm |
Comparative example 1: rectification purification of tetra (dimethylamino) titanium
The low-purity tetra (dimethylamino) titanium is rectified, the fraction with the temperature of 50 ℃/0.1mmHg is collected, and the purity of the product is 99.9454 percent by ICP detection.
Comparative example 2: rectification purification of tetra (methylethylamino) titanium
The low-purity tetra (methylethylamino) titanium is rectified, the fraction with the temperature of 78 ℃/0.1mmHg is collected, and the purity of the product is 99.9689 percent by ICP detection.
Comparative example 3: rectification purification of tetra (methylethylamino) zirconium
The low-purity zirconium tetra (methylethylamino) is rectified, the fraction of 81 ℃/0.1mmHg is collected, and the purity of the product is 99.9326 percent by ICP detection.
Comparative example 4: rectification purification of tetra (diethylamino) hafnium
The low-purity hafnium tetra (diethylamino) was distilled, and 130 ℃/0.1mmHg fractions were collected and tested by ICP to obtain 99.6651% purity.
The ICP measurement results of the above examples and comparative examples are shown in the following table 5:
TABLE 5 ICP measurement results
From the above, it can be seen that the purity of the crude tetrakis (dimethylamino) titanium, tetrakis (methylethylamino) zirconium and tetrakis (diethylamino) hafnium obtained by distillation only reaches 99.9%; after the rectified product is purified by a purification tower filled with a polyethylene porous particle purification material, the purity of the obtained product is as high as 99.9999 percent, so that the purification method can greatly improve the purity of the product, and the product can meet the purity requirement of the ALD precursor material.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (10)
1. A method for refining a liquid ALD precursor, comprising the steps of:
rectifying a crude product of the liquid ALD precursor;
pretreating the purification material, and filling the purification tower with the pretreated purification material;
flowing the rectified components into a purification tower filled with purification materials, carrying out purification treatment at a boiling point temperature, and discharging after purification to obtain a high-purity ALD precursor;
the purification material is porous particles, the porous particles are provided with through pore channels with hollow bending structures, and the pore channels are provided with a plurality of U-shaped bends; the boiling point temperature is the boiling point temperature of the liquid ALD precursor in a decompression state, and the boiling point temperature range is 50-120 ℃; the high purity is a purity higher than 99.9999%.
2. The method of claim 1, wherein the liquid ALD precursor is one of tetrakis (dimethylamino) titanium, tetrakis (dimethylamino) hafnium, tetrakis (methylethylamino) titanium, tetrakis (methylethylamino) zirconium, tetrakis (methylethylamino) hafnium, tetrakis (diethylamino) titanium, tetrakis (diethylamino) zirconium, and tetrakis (diethylamino) hafnium.
3. The method as claimed in claim 1, wherein the purification material has a mesh size of 100-200.
4. A method of refining a liquid ALD precursor according to claim 1 or 3, characterized in that the purification material is ultra high molecular weight polyethylene porous particles.
5. The method as claimed in claim 4, wherein the molecular weight of the porous particles of UHMWPE is 1500000-3000000, and the distribution index of the molecular weight is 1.1-1.7.
6. The method of claim 4, wherein the porous particles of UHMWPE have a diameter of 3-5mm and a pore size of 0.5-1 μm.
7. The method as claimed in claim 4, wherein the porous particles of UHMWPE have a melting point of 200-220 ℃.
8. A method for refining a liquid ALD precursor as recited in claim 1, wherein the pre-treatment of the purification material is specifically: washing the purified material with ultrapure water, and drying the washed purified material to obtain a pretreated purified material; the temperature of the drying treatment is 110-150 ℃, and the time of the drying treatment is 12-36 h.
9. The method for refining the liquid ALD precursor, as recited in claim 1, wherein the purification tower consists of a heating device, a feed valve, a tower body and a discharge valve in sequence from bottom to top; the tower body is used for containing purification materials, and the heating device is used for heating the materials at the bottom of the tower body; the tower body is provided with a heat insulation layer.
10. A method of refining a liquid ALD precursor according to claim 1, characterized in that the time of the purification process is 3-9 h.
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