CN108300980B - X-ray zone plate preparation system - Google Patents

Abstract

The invention relates to an X-ray zone plate preparation system. The system comprises: a chamber; the first precursor introducing pipeline is communicated with one end of the chamber and is used for conveying the first precursor into the chamber; the second precursor introducing pipeline is communicated with one end of the chamber and is used for conveying a second precursor into the chamber; the clamp is arranged in the cavity and used for fixing the columnar filament-shaped substrate; the muffle furnace wraps the cavity and is used for heating the cavity; one end of the air pumping pipeline is communicated with the other end of the cavity; and the vacuum pump is connected with the other end of the air pumping pipeline and pumps the inside of the cavity into vacuum through the air pumping pipeline. The invention can realize the alternate growth of two zone plate materials on a plurality of columnar filament-shaped substrates at the same time, and improve the processing efficiency of the zone plate.

Description

An X-ray zone plate preparation system

technical field

The invention relates to the technical field of atomic layer deposition, in particular to an X-ray zone plate preparation system.

Background technique

Atomic layer deposition (ALD) is a thin film preparation technology that can achieve single atomic layer growth. Its self-limitation and complementarity allow this technology to have excellent control over the composition and thickness of the thin film, and the prepared thin film has good conformality. , high purity and uniform, has been widely used in various fields.

At present, the preparation of X-ray zone plates by atomic layer deposition technology is an effective method to improve the resolution and diffraction efficiency of X-ray zone plates. The X-ray zone plate is an optical element in the X-ray band, which has the functions of dispersion, focusing and imaging of X-rays. The traditional preparation methods mainly include laser holography, electron beam lithography, sputtering sectioning, etc. These traditional manufacturing methods can only make the width of the outermost ring of the zone plate about 20nm. At the same time, the aspect ratio of the laser holography method and the electron beam lithography method is limited in the production of the zone plate, and the sputtering slicing method is very difficult. It is difficult to precisely control the width of each ring of the zone plate. Therefore, it is difficult to realize the fabrication of high-resolution and high-diffraction-efficiency zone plates by traditional methods.

Using ALD technology to prepare the zone plate can precisely control the width of each ring of the zone plate, and the thickness uniformity is high. At the same time, the width of the outermost ring can be controlled below 10nm, and the sub-10nm high resolution can be achieved. However, slicing and polishing with FIB can obtain any aspect ratio, so that the zone plate has high diffraction efficiency.

As shown in Fig. 1, in the equipment chamber 1 of the conventional ALD, a uniform heating plate 3 is generally provided above the heating plate 2. This traditional ALD equipment chamber can only heat the sheet-like substrate. When the target substrate is filamentous, this ALD equipment chamber does not have a fixture for fixing the metal filament, so the filamentous shape cannot be realized. Growth of material on a substrate.

SUMMARY OF THE INVENTION

The object of the present invention is to provide an X-ray zone plate preparation system, which can grow the zone plate material on the filamentous substrate, so that the processing efficiency is greatly improved.

In order to solve the above technical problems, the present invention provides an X-ray zone plate preparation system, the system includes: a chamber; a first precursor inlet pipeline, the first precursor inlet pipeline and the chamber One end of the first precursor is connected to the chamber for transporting the first precursor into the chamber; the second precursor is introduced into the pipeline, and the second precursor inlet pipeline is communicated with one end of the chamber and is used to transfer the second precursor The body is transported into the chamber; a jig, which is arranged in the chamber, is used for fixing the substrate in the shape of a columnar filament; a muffle furnace, which wraps the chamber and is used for heating the chamber; an air extraction pipeline, one end of the air extraction pipeline is connected to the other end of the chamber; a vacuum pump, the vacuum pump is connected to the other end of the air extraction pipeline, and the vacuum pump passes through the air extraction pipeline The circuit draws a vacuum inside the chamber.

Further, the clamp includes: a hollow cylindrical frame, the hollow cylindrical frame includes a first annular end, a second annular end and a connecting rod, the first annular end and the second annular end are relatively parallel to each other, the The first annular end and the second annular end are respectively fixed on both ends of the connecting rod; the axial direction of the hollow cylindrical frame is consistent with the direction of the airflow of the first precursor and the second precursor; several The hooks are symmetrically arranged on the first annular end and the second annular end; the two ends of the cylindrical filament-shaped substrate are respectively fixed on a pair of symmetrical hooks.

Further, the material of the clamp is one of stainless steel, aluminum, copper, and tungsten.

Further, the chamber is a cylindrical tubular structure, the first precursor and the second precursor flow in a unidirectional straight line in the chamber, and the longitudinal direction of the substrate is along the first precursor body and the direction of the gas flow of the second precursor.

Further, the chamber is a quartz tube, the wall thickness of the quartz tube is 2-5 mm, the tube length is 0.8-2 m, and the inner diameter is 1-5 cm.

Further, the outer diameter of the first annular end and the second annular end is 5mm smaller than the inner diameter of the quartz tube.

Further, the heating temperature of the muffle furnace is 50-1200°C.

Further, the system further includes: a vacuum gauge, which is arranged on the air extraction pipeline and is used to measure the vacuum degree in the chamber in real time.

Further, the material of the clamp is one of stainless steel, aluminum, copper, and tungsten.

The technical scheme provided by the present invention has the following technical effects or advantages:

1, the present invention adopts a clamp to fix the substrate of the columnar filament shape, and can realize the alternate growth of two kinds of zone plate materials on the substrate of this shape;

2. The chamber of the present invention adopts a columnar tubular structure, and one end of the columnar tubular structure is set in the precursor inlet pipeline of the two precursors to realize the unidirectional flow of the precursor gas flow. The longitudinal direction of the columnar filament substrate is along the The direction of the precursor gas flow shortens the process purge time;

3. In the present invention, a muffle furnace is used to wrap the chamber to maintain a constant temperature of the substrate;

4. The material of the fixture in the present invention adopts stainless steel, aluminum, copper, tungsten, etc., which has good thermal conductivity and small thermal expansion coefficient, which is beneficial to conduct heat conduction to the substrate fixed on the fixture.

Description of drawings

In order to explain the embodiments of the present invention or the technical solutions in the prior art more clearly, the following briefly introduces the accompanying drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only It is an embodiment of the present invention. For those of ordinary skill in the art, other drawings can also be obtained according to the provided drawings without creative work.

FIG. 1 is a schematic structural diagram of an X-ray zone plate preparation system according to an embodiment of the present invention.

FIG. 2 is a wire clamp provided by an embodiment of the present invention.

Detailed ways

In order to make the purposes, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments These are some embodiments of the present invention, but not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work, all belong to the protection scope of the present invention.

As shown in FIG. 1, an embodiment of the present invention provides an X-ray zone plate preparation system, the system includes: a chamber 3; a first precursor inlet pipeline 1, the first precursor inlet pipeline 1 and One end of the chamber 3 is connected to the chamber 3 for delivering the first precursor; One end is connected to transport the second precursor into the chamber 3; a fixture 4, the fixture 4 is arranged in the chamber 3 and used to fix the columnar filament-shaped substrate 9; a muffle furnace 5 , the muffle furnace 5 wraps the chamber 3 and is used to heat the chamber 3; an air extraction pipeline 6, one end of the air extraction pipeline 6 is communicated with the other end of the chamber 3; a vacuum pump 8 , the vacuum pump 8 is connected to the other end of the air extraction pipeline 6 , and the vacuum pump 8 evacuates the chamber 3 to a vacuum through the air extraction pipeline 6 .

In this embodiment, the chamber 3 is a cylindrical tubular structure, the first precursor and the second precursor flow in a unidirectional straight line in the chamber 3 , and the longitudinal direction of the substrate 9 is along the direction of the airflow of the first precursor and the second precursor.

In this embodiment, as shown in FIG. 2 , the clamp includes: a hollow cylindrical frame, the hollow cylindrical frame includes a first annular end 41 , a second annular end 42 and a connecting rod 43 , the first annular end 41 and the The second annular end 42 is relatively parallel to each other, and the first annular end 41 and the second annular end 42 are respectively fixed on both ends of the connecting rod 43; A precursor and the second precursor flow in the same direction; a plurality of hooks 44 are symmetrically arranged on the first annular end 41 and the second annular end 42 ; a cylindrical filament-shaped lining Both ends of the bottom 9 are respectively fixed on a pair of symmetrical hooks 44 .

In this embodiment, a tungsten wire with a diameter of 30 μm is selected as the substrate, the two ends of the tungsten wire are wound on the toothed structure of the fixture 4 respectively, and Kapton tape is used to fix both ends of the tungsten wire, and the longitudinal direction of the tungsten wire is along the flow of the precursor airflow. direction.

In this embodiment, the material of the clamp 4 is stainless steel, aluminum, copper, tungsten and other metals. Stainless steel is preferred in this embodiment.

In this embodiment, the chamber 3 is a quartz tube, the wall thickness of the quartz tube is 2-5mm, the tube length is 0.8-2m, the inner diameter is 1-5cm, and the high temperature resistance can reach 1200°C. The outer diameter of the first annular end 41 and the second annular end 42 is 5 mm smaller than the inner diameter of the quartz tube.

In this embodiment, the heating temperature of the muffle furnace 5 is 50-1200°C.

In this embodiment, the system further includes: a vacuum gauge 7, which is arranged on the air extraction pipeline 6 and is used to measure the vacuum degree in the chamber 3 in real time.

The working process of the embodiment of the present invention is as follows:

A plurality of tungsten wires are fixed in the chamber 3 through the fixture 4, so that the longitudinal direction of the tungsten wires is consistent with the flow direction of the precursor; the vacuum pump 8 is turned on, and the vacuum degree in the chamber 3 is measured in real time through the vacuum gauge 7. When the vacuum degree in the chamber reaches As required, the precursor is introduced into the chamber 3 . The two types of zone plate materials deposited in the embodiments of the present invention are thin-film laminated materials, and the other is a material with high X-ray transmittance, such as C, Al, Al ₂ O ₃ , Si ₃ N ₄ , etc., preferably Alumina, another material with low X-ray transmittance, such as Ag, Cu, Ni, Ir, SiO ₂ , Ta ₂ O ₅ , HfO ₂ , etc., preferably HfO ₂ , Ta ₂ O ₅ . The two selected materials are respectively transported into the chamber 3 through the first precursor inlet pipeline 1 and the second precursor inlet pipeline 2. Since the process temperature of the selected two precursor materials is 200 °C, it needs to be used as The temperature of the tungsten wire of the substrate is maintained at a constant temperature of 200°C; at this time, the muffle furnace 5 is used to maintain the constant temperature of 200°C of the tungsten wire, and the two precursors alternately grow the zone plate material on the tungsten wire substrate.

One or more technical solutions provided in the embodiments of the present invention have at least the following technical effects or advantages:

1, the present invention adopts a fixture to fix the substrate of a plurality of columnar filaments, and can realize the alternate growth of two kinds of zone plate materials on the substrate of this shape, and improve the processing efficiency of the zone plate;

2. The chamber of the present invention adopts a columnar tubular structure, and one end of the columnar tubular structure is set in the precursor inlet pipeline of the two precursors to realize the unidirectional flow of the precursor gas flow. The longitudinal direction of the columnar filament substrate is along the The direction of the precursor gas flow shortens the process purge time;

3, in the present invention, adopt the muffle furnace to wrap the chamber, maintain the constant temperature of the substrate, and precisely control the growth thickness of the film;

4. The material of the fixture in the present invention adopts stainless steel, which has good thermal conductivity and small thermal expansion coefficient, which is beneficial to conduct heat conduction to the substrate fixed on the fixture.

Although preferred embodiments of the present invention have been described, additional changes and modifications to these embodiments may occur to those skilled in the art once armed with the basic inventive concepts. Therefore, the appended claims are intended to be construed to include the preferred embodiment and all changes and modifications that fall within the scope of the present invention.

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 and scope of the invention. Thus, provided that these modifications and variations of the present invention fall within the scope of the claims of the present invention and their technical equivalents, the present invention is also intended to include these modifications and variations.

Claims (6)

1. An X-ray zone plate preparation system, the system comprising:

a chamber;

the first precursor introducing pipeline is communicated with one end of the chamber and is used for conveying a first precursor into the chamber;

the second precursor introducing pipeline is communicated with one end of the chamber and is used for conveying a second precursor into the chamber;

a clamp disposed within the chamber for securing a cylindrical filament-shaped substrate;

a muffle enclosing the chamber for heating the chamber;

one end of the air pumping pipeline is communicated with the other end of the cavity;

the vacuum pump is connected with the other end of the air pumping pipeline and pumps the inside of the cavity into vacuum through the air pumping pipeline;

wherein, the anchor clamps include:

the hollow cylindrical frame comprises a first annular end, a second annular end and a connecting rod, the first annular end and the second annular end are arranged in parallel relatively, and the first annular end and the second annular end are respectively fixed at two ends of the connecting rod; the axial direction of the hollow cylindrical frame is consistent with the direction of the gas flow of the first precursor and the second precursor;

the hooks are symmetrically arranged on the first annular end and the second annular end; two ends of the columnar filament-shaped substrate are respectively fixed on the pair of symmetrical hooks;

the chamber is of a columnar tubular structure, the first precursor and the second precursor flow linearly in the chamber in a unidirectional mode, and the longitudinal direction of the substrate is along the direction of gas flows of the first precursor and the second precursor.

2. The manufacturing system of claim 1, wherein: the clamp is made of one of stainless steel, aluminum, copper and tungsten.

3. The manufacturing system of claim 1, wherein: the chamber is a quartz tube, the wall thickness of the quartz tube is 2-5mm, the length of the quartz tube is 0.8-2m, and the inner diameter of the quartz tube is 1-5 cm.

4. The manufacturing system of claim 3, wherein: the outer diameter of the first annular end and the second annular end is 5mm smaller than the inner diameter of the quartz tube.

5. The manufacturing system of claim 1, wherein: the heating temperature of the muffle furnace is 50-1200 ℃.

6. The manufacturing system of claim 1, wherein: the system further comprises: and the vacuum gauge is arranged on the air exhaust pipeline and is used for measuring the vacuum degree in the cavity in real time.

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