WO2021227184A1 - Process for manufacturing grating by adhering heavy-metal colloid to light-metal film - Google Patents

Process for manufacturing grating by adhering heavy-metal colloid to light-metal film Download PDF

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Publication number
WO2021227184A1
WO2021227184A1 PCT/CN2020/095996 CN2020095996W WO2021227184A1 WO 2021227184 A1 WO2021227184 A1 WO 2021227184A1 CN 2020095996 W CN2020095996 W CN 2020095996W WO 2021227184 A1 WO2021227184 A1 WO 2021227184A1
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WIPO (PCT)
Prior art keywords
heavy metal
metal film
light
film
light metal
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PCT/CN2020/095996
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French (fr)
Chinese (zh)
Inventor
郭金川
宗方轲
杨君
吴浩
罗琨皓
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深圳大学
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Publication of WO2021227184A1 publication Critical patent/WO2021227184A1/en

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    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00Optical elements other than lenses
    • G02B5/18Diffraction gratings
    • G02B5/1847Manufacturing methods
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00Layered products comprising a layer of metal
    • B32B15/01Layered products comprising a layer of metal all layers being exclusively metallic
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B32B37/1284Application of adhesive
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B43/00Operations specially adapted for layered products and not otherwise provided for, e.g. repairing; Apparatus therefor
    • B32B43/003Cutting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04Interconnection of layers
    • B32B7/12Interconnection of layers using interposed adhesives or interposed materials with bonding properties

Definitions

  • the invention relates to the technical field of optical elements, in particular to a grating manufacturing process in which a light metal film adheres to a heavy metal colloid.
  • X-ray imaging technology has been rapidly developed as a brand new discipline since the German researcher Roentgen discovered X-ray in 1895. It can detect internal defects of welds and equipment, and is widely used in machinery manufacturing, pressure vessels, and aviation. Aerospace, petroleum, chemical, railway transportation, metallurgy, shipbuilding, military industry and other industrial sectors; the current process of making gratings mainly uses DRIE technology, LIGA technology and silicon-based photo-assisted electrochemical etching technology.
  • DRIE is an anisotropic dry etching technology, which is based on inductively coupled plasma for deep processing of silicon or other materials; firstly, the mask is covered on the substrate to be etched, and an appropriate gas is filled for etching. However, lateral corrosion will follow in this process, so after a certain depth of etching, a layer of polymer is deposited on the etched surface to form a sidewall protective film. The protective film needs to be worn off before the silicon can continue to be etched. .
  • the X light source requires an expensive accelerator, which is costly, and the mask used for X-ray lithography is itself a 3D microstructure, which is complicated to produce and has a long period.
  • LIGA processing technology is one of the traditional manufacturing methods of absorption grating 7 and is often used to produce gratings with large aspect ratio structures.
  • the principle of LIGA technology is to combine lithography (Lithographie), electroforming (Galvanoformung) and injection molding (Abformung). These three are combined.
  • lithography Lithographie
  • electroforming Gavanoformung
  • Abformung injection molding
  • the photo-assisted electrochemical etching method has a complicated process, and the silicon-based resistivity, temperature, etching solution, etc. all have a greater impact on the etching structure during the production process, which is difficult to control.
  • the required filling process is complicated and the conditions are relatively harsh.
  • the present invention provides a manufacturing process for grating 7 with light metal film 1 adhered to heavy metal colloid.
  • the light metal film 1 to which heavy metal colloid solution is attached is directly stacked with the light metal film 1 to which heavy metal colloid solution is not attached.
  • a composite film stack of light and heavy metals is formed, and finally cut and packaged to obtain the grating 7; the entire process grating 7 has a short production cycle, low cost, and a convenient and quick production process.
  • the present invention provides a manufacturing process for grating 7 with light metal film 1 adhering heavy metal colloid, including
  • Preparation of heavy metal colloid solution adding a dispersant and a reducing agent to the heavy metal salt solution in order to obtain a heavy metal colloid solution;
  • Add adhesive add adhesive to the prepared heavy metal colloid solution to obtain a viscous heavy metal colloid solution
  • Making the viscous light metal film 1 transfer the light metal film 1 to the viscous heavy metal colloid solution, so that the heavy metal particles adhere to the light element metal plate, and then transfer the light metal film 1 out to obtain the viscous light metal film 1;
  • Making a composite film stack stack the light metal film 1 and the viscous light metal film 1 on each other to obtain a composite film stack;
  • the composite film stack is cut according to the set size to obtain the quasi-grating 5;
  • the quasi-grating 5 is packaged with a weak X-ray absorbing material to obtain the grating 7.
  • the heavy metal colloidal solution when preparing the heavy metal colloidal solution, first add concentrated ammonia water to the heavy metal salt solution to obtain the metal ammonia complex solution, then add the dispersant to the metal ammonia complex solution, and after stirring uniformly, add the reducing agent dropwise, After being evenly stirred, a nano-scale heavy metal colloid is obtained.
  • the molar ratio of the heavy metal salt to the dispersant is 11:1-12:1.
  • the molar ratio of the heavy metal salt to the reducing agent is 1:3-1:5.
  • the adhesive when the adhesive is added, the adhesive is a heat-volatile adhesive.
  • the heavy metal layer 2 is adhered to both sides of the light metal film 1; the thickness of the heavy metal layer 2 is controlled by controlling the concentration of the heavy metal colloid solution.
  • the adhesive light metal film 1 and the light metal film 1 are folded alternately or directly rolled up to form a composite film stack in which the light metal film 1 and the heavy metal layer 2 are stacked at intervals.
  • the edge of the composite membrane stack is first cut to obtain the composite membrane stack of the first shape, and then the composite membrane stack of the first shape is cut according to the set size to obtain the quasi grating 5.
  • the cut surface of the quasi-grating 5 is clamped by the carbon fiber 6 material plate until the carbon fiber 6 adheres to the composite films to complete the packaging.
  • the process of the present invention includes: preparing a heavy metal colloid solution, adding an adhesive, adhering to the heavy metal colloid solution, making a composite film laminate, cutting and encapsulating; five major steps, firstly preparing a heavy metal colloid by heavy metal salt , And then add a heating and volatile adhesive to the heavy metal colloid to increase the viscosity of the heavy metal colloid, and then pass the light metal film through the viscous heavy metal colloid to obtain two adhesive light metal films that adhere to the heavy metal layer, and then combine the light metal film and the adhesive
  • the flexible light metal film is folded alternately to obtain a composite film stack, and finally the composite film stack is cut and encapsulated to obtain a grating 7.
  • the whole production process of the present invention is short, the cost price is low, and the production process is convenient and quick.
  • the fabricated structure will not collapse.
  • By controlling the width of the light element metal sheet it can be used to fabricate gratings of any area. Through one fabrication, X-ray gratings can be mass-produced.
  • Figure 1 is a process flow diagram of the present invention
  • Figure 2 is a schematic diagram of the directly purchased metal film drum structure
  • FIG. 3 is a schematic diagram of the light metal film of the present invention obtained by physical rolling technology to obtain a predetermined thickness
  • FIG. 4 is a schematic diagram of the light metal film of the present invention forming a viscous light metal film 1;
  • FIG. 5 is a schematic diagram of the first step of stacking the adhesive light metal film and the light metal module of the present invention.
  • FIG. 6 is a schematic diagram of the second step of stacking the adhesive light metal film and the light metal module of the present invention.
  • FIG. 7 is a schematic diagram of the third step of stacking the adhesive light metal film and the light metal module of the present invention.
  • FIG. 8 is a schematic diagram of the sticky light metal film block and the light metal module stack of the present invention.
  • FIG. 9 is a schematic view of the sticky light metal film and the light metal mold being vertically rolled and stacked according to the present invention.
  • FIG. 10 is a schematic diagram of the roll of the viscous light metal film of the present invention.
  • FIG. 11 is a schematic diagram of the quasi-grating 5 obtained by cutting the first shape composite film stack 4 of the present invention.
  • FIG. 12 is a schematic diagram of the first-shaped composite membrane stack 4 according to the present invention.
  • Figure 13 is a schematic diagram of the quasi-grating structure of the present invention.
  • Fig. 14 is a schematic diagram of the grating structure of the present invention.
  • the characteristics are: bright stripes are very bright and narrow, the dark area between adjacent bright stripes is very wide, and the diffraction pattern is very clear; if the deviation of the slit width and the slit spacing is too large due to manufacturing errors, the image will be blurred during diffraction , The final image obtained by X-rays will be blurred and unclear; especially in medical applications, unclear images can easily lead to a very high error rate in disease inspection; therefore, how to
  • the current process for making grating 7 mainly includes DRIE technology, LIGA technology and silicon-based photo-assisted electrochemical etching technology; in the process of making grating 7 by DRIE technology, the X light source requires expensive accelerators, and the cost is high.
  • the mask used for X-ray lithography is itself a 3D microstructure with a long production cycle; in the LIGA technology, when the grating 7 is produced, the grating 7 often breaks and collapses and causes structural failure.
  • the production cost is relatively high, and the production area is small; the photo-assisted electrochemical etching method has a complicated process, and the silicon-based resistivity, temperature, and etching solution during the production process have a large impact on the etching structure, which is difficult to control.
  • the required filling process is complicated and the conditions are relatively harsh; currently, there has not yet been a low cost, short cycle, convenient manufacturing process and suitable for mass production of the grating 7 manufacturing process.
  • the present application provides a manufacturing process for grating 7 with light metal film 1 adhered to heavy metal colloid. Please refer to FIG. 1, which includes the following steps:
  • Add adhesive add adhesive to the prepared heavy metal colloid solution to obtain a viscous heavy metal colloid solution
  • Adhesive heavy metal colloid solution transfer the light metal film 1 to the viscous heavy metal colloid solution, so that the heavy metal particles adhere to the light element metal plate and then transfer the light metal film 1 out to obtain the adhesive light metal film 1;
  • the composite film stack is cut according to the set size to obtain the quasi-grating 5;
  • the quasi-grating 5 is packaged with a weak X-ray absorbing material to obtain the grating 7.
  • the heavy metals can be metals with large atomic numbers such as tungsten, silver, lead, gold; the corresponding heavy metal salt solutions include lead acetate solution, nitrate solution, gold trichloride solution, etc.; the solution can be purchased directly from the market
  • the corresponding powder can be obtained by directly dissolving in water; after obtaining the metal salt solution, first add concentrated ammonia water to the metal salt solution to obtain a metal ammonia complex solution; wherein the concentration of ammonium ions in the concentrated ammonia water is greater than 15%; dispersant Including alkali metal phosphates, such as: sodium tripolyphosphate, sodium hexametaphosphate and sodium pyrophosphate, lauric acid, triethylhexyl phosphoric acid, sodium lauryl sulfate, methylpentanol, cellulose derivatives, poly Acrylamide, Guer gum, fatty acid polyethylene glycol ester, etc.; dissolve the complex after adding dispersant; after the complex is
  • the molar ratio of the heavy metal salt to the dispersant is 11:1-12:1, preferably 11.6:1.
  • the molar ratio of the heavy metal salt to the reducing agent is 3:1-5:1; preferably 4:1.
  • the adhesive when the adhesive is added, the adhesive is a heat-volatile adhesive; the adhesive includes bisphenol A type, novolac type, novolac epoxy resin, polyurethane adhesive, etc.; preferably Adopt: ethyl acrylate as adhesive.
  • the heavy metal layer 2 is adhered to both sides of the light metal film 1; the thickness of the heavy metal layer 2 is controlled by controlling the particle concentration of the heavy metal colloid.
  • the light metal material is a metal with a small atomic number such as aluminum or beryllium; usually the prefabricated light metal film 1 has a thickness of 50-80 microns; a width of about 5-10 cm; it is wound on a roller like a roll of paper Above; the light metal film 1 is made through a drawing and pressing process, and there are finished products on the market for direct sale; the light metal film 1 is prefabricated, and the production of the light metal film 1 is separated from the production of the grating 7 to provide an independent environment for each process , It is more conducive to mass production of the assembly line; and the size of the light metal film 1 can be preset to better control the accuracy, so that the error in the production of the grating 7 is smaller.
  • the prefabricated light metal film 1 has a thickness of 50-80 microns; a width of about 5-10 cm; it is wound on a roller like a roll of paper Above; the light metal film 1 is made through a drawing and pressing process, and there are finished products on the market for direct sale;
  • the light metal film 1 is pulled out of the roller before being transferred to the heavy metal colloid solution, and after being pulled out, it is transported through the rolling equipment, and the rolling equipment rolls the thickness of the light metal film 1 to the set value.
  • the setting value is 30 microns
  • the thickness of the light metal film 1 is rolled from 60 microns to 30 microns.
  • the light metal film 1 has heavy metal particle layers adhered on both sides to form an adhesive light metal film 1.
  • the thickness of the heavy metal layer 2 is determined by the particle solubility of the colloid; for example, the solubility of the heavy metal colloid is 15.2g/L, and the light metal film 1 The time to pass through the heavy metal colloid is 1 min, and the heavy metal layer 2 with a thickness of 25 microns is formed on both sides of the light metal film 1.
  • the light metal film 1 is drawn from the roller, rolled, and then transferred to the viscous heavy metal colloid solution and passed out.
  • the light metal film 1 can be a long strip that has not been broken, or it can be First pull off the light metal film 1 from the drum, and then pass through the rolling equipment and viscous heavy metal colloid in sequence; for example, after the light metal film 1 is pulled from the drum, it is cut into a piece of light metal film with a length of 10 cm, a width of 5 cm and a thickness of 60 microns. Then pass the roller 11, and follow-up processing in turn.
  • the viscous light metal film 1 can also be obtained by directly spraying heavy metal colloid on the light metal film 1.
  • the light metal is first pulled out of the roller and then passed through a rolling device, which rolls the thickness of the light metal film 1 Press to the set value; then directly spray heavy metal colloid on both sides of the light metal film 1.
  • the adhesive light metal film 1 needs to be heated to volatilize the adhesive liquid, and the heavy metal particles are solidified on the light element metal surface to finally obtain the adhesive light metal film 1.
  • the thickness of the heavy metal layer 2 does not change during the volatilization of the adhesive liquid; after being transferred from the viscous heavy metal colloid, the adhesive liquid is volatilized by a constant temperature heating device, and the heavy element metal particles are solidified on the light element metal surface at a constant temperature.
  • the temperature and heating time are different depending on the type of adhesive added; for example: the adhesive is ethyl acrylate as the adhesive, the heating time is 10min, the heating temperature is 80 degrees, the adhesive liquid is completely volatilized, heating The thickness of the front heavy metal layer 2 is 25 microns, and the thickness of the heavy metal layer 2 is still 25 microns after heating.
  • the light metal film 1 and the viscous light metal film 1 are folded alternately to form a composite film stack in which the light metal film 1 and the heavy metal layer 2 are stacked at intervals.
  • the thickness D of the single light metal film 1 and the heavy metal film on its surface The sum of the layer thickness d is the period n of the grating 7.
  • the viscous light metal film 1 is a long strip that has not been broken.
  • the light metal film 1 is pre-cut into a light metal film of a predetermined shape and size, such as a light metal module with a length of 10 cm, a width of 6 cm, and a thickness of 30 microns;
  • the width of the light metal is 6cm, the thickness is 30 microns, and the thickness of the heavy metal layer 2 on the viscous light metal is 50 microns; with the light metal film 1 as the bottom layer, a layer of viscous light metal film 1 is covered on the light metal film 1, and then on the viscous light metal film 1.
  • the grating 7 period is 80 microns; among them, the alternate stacking adopts the zigzag stacking method, which has high stacking efficiency; the two opposite sides of the composite film stack will be curled due to the viscous metal film The resulting connection portion 13.
  • Both the light metal film 1 and the viscous light metal film 1 are pulled into pieces of metal film of a set size, and one piece of light metal film is cut into a piece of light metal film of a set shape and size after passing through the rolling equipment, for example, cut into a length of 10cm ,
  • a viscous light metal module with a width of 6cm and a thickness of 30 microns.
  • the thickness of the heavy metal layer 2 on the viscous light metal is 50 microns; the size of the light metal film 1 is exactly the same as the size of the viscous light metal; the light metal film 1 is directly connected to the viscous metal module.
  • Interleaved stacked to form a composite film stack; the grating 7 has a period of 80 microns.
  • the light metal film 1 and the viscous light metal film 1 are both long and unbroken.
  • the size of the light metal and the viscous light metal are both 6cm in width and 30 microns in thickness, and the thickness of the heavy metal layer 2 is 50 microns; 1.
  • Place the adhesive metal film in the first direction place the adhesive metal film in the second direction, the first direction and the second direction are perpendicular to each other; interfold the light metal film 1 and the adhesive light metal film 1 to form a composite film stack with a length and a width of 6 cm;
  • the 7 period is 80 micrometers; and the adjacent surface of the grating 7 will have a connection portion 13 due to the bending of the viscous metal film and the light metal film 1.
  • the viscous light metal film 1 is a long strip that is not broken.
  • the size of the viscous light metal film 1 is 6cm in width, 30 microns in thickness, and the heavy metal layer 2 is 50 microns in thickness; Set the length and fold back and forth to obtain a composite membrane stack with light metal film 1 and heavy metal layer 2 staggered.
  • the period of the grating 7 in the composite membrane stack is 130 microns;
  • the connecting portion 13 produced by the bending of the film 1.
  • the composite membrane stack after removal is preferably a rectangular parallelepiped; laser resection or wire cutting machine or milling cutter is used for resection; preferably High-power laser cutting, the precision can reach 0.01mm during cutting.
  • the first shape may be a polygon, a rectangle, a triangle or other shapes; the preferred first shape is a rectangle.
  • the first shape is cut along the width direction of the composite film stack to obtain a plurality of quasi gratings 5, and the thickness direction of the first shape is the width of the quasi grating 5 ,
  • the width direction of the first shape is the length direction of the quasi grating 5;
  • the cutting pitch is the thickness direction of the quasi grating 5;
  • the length of the grating 7 obtained after cutting is the same; the thickness direction of the grating 7 does not need to be cut during the entire cutting process, And only the number of cuts is small, and the production precision is high.
  • the cutting direction and angle when cutting the first shape, the cutting direction and angle can be adjusted arbitrarily, and after cutting, it is not limited to vertical cutting.
  • the carbon fiber 6 material film is used to clamp the cut surface in the width direction of the first shape until the carbon fiber 6 adheres to the composite film of each layer to complete the packaging, and the grating 7 is obtained.
  • the light metal film 1 can be compressed to a predetermined thickness D by physical rolling technology, and then the light metal film 1 can be passed through a heavy metal colloid to obtain a viscous light metal film 1 of a set size;
  • the production cycle of the grating 7 produced by the present invention is short, the cost is low, and the production process is convenient and quick; the produced structure will not collapse, and the grating 7 of any area can be produced by controlling the width of the light element metal plate. Through one production, X-ray grating 7 can be produced in large quantities.
  • the composite film stack Before the light metal film 1 is made into a composite film stack, normal processing may not be performed, and the composite film stack can be stacked to form a composite film stack and then cut.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Laminated Bodies (AREA)

Abstract

Disclosed is a process for manufacturing a grating (7) by adhering a heavy-metal colloid to a light-metal film (1), which process relates to the field of optical elements. The manufacturing process comprises five main steps: preparing a heavy-metal colloid solution, adding a binder therein, adhering the heavy-metal colloid solution, manufacturing a composite film laminate, and cutting and packaging; and specifically involves: first preparing a heavy-metal salt to obtain a heavy-metal colloid; then adding the binder, which is easy to volatilize by means of heating, into the heavy-metal colloid to increase the viscosity of the heavy-metal colloid; passing a light-metal film (1) through the viscous heavy-metal colloid to obtain an adhesive light-metal film (1) with heavy-metal layers (2) adhered on two faces thereof; then alternating and folding the light-metal film (1) and the adhesive light-metal film (1) to obtain a composite film stack; and finally cutting and packaging the composite film stack to obtain a grating (7). The grating (7) has a short manufacturing cycle, is low cost, and has a convenient and quick manufacturing process. The manufactured structure does not collapse, a grating (7) of any area is manufactured by controlling the width of a light-metal plate, and an X-ray grating (7) can be mass produced via one instance of manufacturing.

Description

轻金属膜粘附重金属胶体的光栅制作工艺Grating manufacturing process with light metal film adhered to heavy metal colloid 技术领域Technical field
本发明涉及光学元件技术领域,具体为一种轻金属膜粘附重金属胶体的光栅制作工艺。The invention relates to the technical field of optical elements, in particular to a grating manufacturing process in which a light metal film adheres to a heavy metal colloid.
背景技术Background technique
X射线成像技术自1895年德国研究员伦琴发现X射线以来便作为一个全新的学科得到了迅速的发展,它可以对焊缝、设备的内部缺陷进行探伤检测,广泛应用于机械制造、压力容器、航空航天、石油、化工、铁路交通、冶金、造船、军工等工业部分;目前制作光栅的工艺主要采用DRIE技术、LIGA技术和硅基光助电化学刻蚀技术。X-ray imaging technology has been rapidly developed as a brand new discipline since the German researcher Roentgen discovered X-ray in 1895. It can detect internal defects of welds and equipment, and is widely used in machinery manufacturing, pressure vessels, and aviation. Aerospace, petroleum, chemical, railway transportation, metallurgy, shipbuilding, military industry and other industrial sectors; the current process of making gratings mainly uses DRIE technology, LIGA technology and silicon-based photo-assisted electrochemical etching technology.
DRIE是一种各向异性的干法刻蚀技术,基于电感耦合等离子对硅或其他材料进行深层加工;首先将掩膜板覆盖于待刻蚀的基底上,充入适当的气体进行刻蚀,但在这个过程中会随之产生侧向腐蚀,所以在刻蚀一段深度后在被刻蚀的表面沉积一层聚合物形成侧壁保护膜,需要将保护膜磨掉,才能继续进行刻蚀硅。制作过程中X光源需要昂贵的加速器,成本高,且用于X光光刻的掩膜板本身就是3D微观结构,制作的复杂,周期长。DRIE is an anisotropic dry etching technology, which is based on inductively coupled plasma for deep processing of silicon or other materials; firstly, the mask is covered on the substrate to be etched, and an appropriate gas is filled for etching. However, lateral corrosion will follow in this process, so after a certain depth of etching, a layer of polymer is deposited on the etched surface to form a sidewall protective film. The protective film needs to be worn off before the silicon can continue to be etched. . During the production process, the X light source requires an expensive accelerator, which is costly, and the mask used for X-ray lithography is itself a 3D microstructure, which is complicated to produce and has a long period.
LIGA加工技术是其中一种传统的吸收光栅7制作方法,常用于制作大深宽比结构的光栅,LIGA技术的原理是将光刻(Lithographie)、电铸成型(Galvanoformung)和注塑(Abformung),这三者结合起来。但是在研究的过程中发现用此方法制作光栅7时经常有光栅7断裂坍塌等引起结构失效的现象发生。且制作成本较高,可制作面积较小。LIGA processing technology is one of the traditional manufacturing methods of absorption grating 7 and is often used to produce gratings with large aspect ratio structures. The principle of LIGA technology is to combine lithography (Lithographie), electroforming (Galvanoformung) and injection molding (Abformung). These three are combined. However, in the process of research, it is found that when the grating 7 is made by this method, the grating 7 often breaks and collapses and causes structural failure. Moreover, the production cost is relatively high, and the production area is small.
光助电化学刻蚀方法则流程复杂,而且制作过程中硅基电阻率、温度、腐蚀液等均对刻蚀结构的影响较大,难以控制,在后期的高原子序数金属填充过程中,所需的填充工艺复杂,条件也较为苛刻。The photo-assisted electrochemical etching method has a complicated process, and the silicon-based resistivity, temperature, etching solution, etc. all have a greater impact on the etching structure during the production process, which is difficult to control. In the later high atomic number metal filling process, The required filling process is complicated and the conditions are relatively harsh.
技术问题technical problem
针对上述技术中存在的不足之处,本发明提供一种轻金属膜1粘附重金属胶体的光栅7制作工艺,将附着有重金属胶体溶液的轻金属膜1与未附着重金属胶体溶液的轻金属膜1直接堆叠形成轻、重金属的复合膜堆,最后切割,封装得到光栅7;整个工艺光栅7制作周期短,成本价格低,制作过程方便快捷。In view of the shortcomings in the above-mentioned technology, the present invention provides a manufacturing process for grating 7 with light metal film 1 adhered to heavy metal colloid. The light metal film 1 to which heavy metal colloid solution is attached is directly stacked with the light metal film 1 to which heavy metal colloid solution is not attached. A composite film stack of light and heavy metals is formed, and finally cut and packaged to obtain the grating 7; the entire process grating 7 has a short production cycle, low cost, and a convenient and quick production process.
技术解决方案Technical solutions
为实现上述目的,本发明提供一种轻金属膜1粘附重金属胶体的光栅7制作工艺,包括In order to achieve the above objective, the present invention provides a manufacturing process for grating 7 with light metal film 1 adhering heavy metal colloid, including
制备重金属胶体溶液:向重金属盐溶液中依次添加分散剂和还原剂得到重金属胶体溶液;Preparation of heavy metal colloid solution: adding a dispersant and a reducing agent to the heavy metal salt solution in order to obtain a heavy metal colloid solution;
添加粘合剂:在制备好的重金属胶体溶液里加入粘合剂得到粘性重金属胶体溶液;Add adhesive: add adhesive to the prepared heavy metal colloid solution to obtain a viscous heavy metal colloid solution;
制作粘性轻金属膜1:将轻金属膜1传送至粘性重金属胶体溶液中,使得重金属颗粒粘附在轻元素金属板上后再将轻金属膜1传送出,得到粘性轻金属膜1;Making the viscous light metal film 1: transfer the light metal film 1 to the viscous heavy metal colloid solution, so that the heavy metal particles adhere to the light element metal plate, and then transfer the light metal film 1 out to obtain the viscous light metal film 1;
制作复合膜叠层:将轻金属膜1和粘性轻金属膜1相互叠合,得到复合膜叠层;Making a composite film stack: stack the light metal film 1 and the viscous light metal film 1 on each other to obtain a composite film stack;
切割:按设定尺寸切割后的复合膜堆,得到准光栅5;Cutting: The composite film stack is cut according to the set size to obtain the quasi-grating 5;
封装:使用X射线弱吸收材料封装准光栅5得到光栅7。Packaging: The quasi-grating 5 is packaged with a weak X-ray absorbing material to obtain the grating 7.
其中,制备重金属胶体溶液时,先向重金属盐溶液中加入浓氨水得到金属氨络合物溶液,再向金属氨络合物溶液中加入分散剂,并搅拌均匀后,逐滴滴加还原剂,搅拌均匀后得到纳米级重金属胶体。Among them, when preparing the heavy metal colloidal solution, first add concentrated ammonia water to the heavy metal salt solution to obtain the metal ammonia complex solution, then add the dispersant to the metal ammonia complex solution, and after stirring uniformly, add the reducing agent dropwise, After being evenly stirred, a nano-scale heavy metal colloid is obtained.
其中,制备重金属胶体溶液时,重金属盐与分散剂的摩尔比为11:1—12:1。Wherein, when preparing the heavy metal colloidal solution, the molar ratio of the heavy metal salt to the dispersant is 11:1-12:1.
其中,制备滴加还原剂时,重金属盐与还原剂的摩尔比为1:3—1:5。Wherein, when preparing the dropping reducing agent, the molar ratio of the heavy metal salt to the reducing agent is 1:3-1:5.
其中,添加粘合剂时,粘合剂为加热易挥发形粘合剂。Among them, when the adhesive is added, the adhesive is a heat-volatile adhesive.
其中,制作粘性轻金属膜1时,轻金属膜1两面均粘附重金属层2;通过控制重金属胶体溶液的浓度控制重金属层2的厚度。Wherein, when the viscous light metal film 1 is made, the heavy metal layer 2 is adhered to both sides of the light metal film 1; the thickness of the heavy metal layer 2 is controlled by controlling the concentration of the heavy metal colloid solution.
其中,制作粘性轻金属膜1时,需要对两面均粘附重金属层2的轻金属膜1进行加热处理,使其粘合剂液体挥发,重金属颗粒固化在轻元素金属表面上。Wherein, when the viscous light metal film 1 is made, it is necessary to heat the light metal film 1 with the heavy metal layer 2 adhered on both sides to volatilize the binder liquid and solidify the heavy metal particles on the surface of the light element metal.
其中,制作复合膜叠层时,将粘性轻金属膜1和轻金属膜1交错折叠或者直接卷叠粘性轻金属膜1,形成轻金属膜1和重金属层2间隔堆叠的复合膜堆。Wherein, when making the composite film laminate, the adhesive light metal film 1 and the light metal film 1 are folded alternately or directly rolled up to form a composite film stack in which the light metal film 1 and the heavy metal layer 2 are stacked at intervals.
其中,先切割复合膜堆的边缘得到第一形状的复合膜堆,再按设定尺寸切割第一形状的复合膜堆,得到准光栅5。Wherein, the edge of the composite membrane stack is first cut to obtain the composite membrane stack of the first shape, and then the composite membrane stack of the first shape is cut according to the set size to obtain the quasi grating 5.
其中,利用碳素纤维6材料板夹持准光栅5的切割面,直至碳素纤维6黏合各复合膜,完成封装。Wherein, the cut surface of the quasi-grating 5 is clamped by the carbon fiber 6 material plate until the carbon fiber 6 adheres to the composite films to complete the packaging.
有益效果Beneficial effect
本发明的有益效果是:本发明的工艺包括:制备重金属胶体溶液、添加粘合剂、粘附重金属胶体溶液、制作复合膜叠层、切割和封装;五大步骤,首先通过重金属盐制备得到重金属胶体,再向重金属胶体中添加加热易挥发的粘附剂增加重金属胶体的粘性,再将轻金属膜通过粘性重金属胶体中得到两层粘附重金属层的粘附性轻金属膜,再将轻金属膜和粘附性轻金属膜交错折叠得到复合膜堆,最后切割、封装复合膜堆得到光栅7。整个本发明制作光栅制作周期短,成本价格低,制作过程方便快捷。制作的结构不会垮塌,通过控制轻元素金属板材的宽度,用来制作任意面积的光栅,通过一次制作,可大批量生产出X射线光栅。The beneficial effects of the present invention are: the process of the present invention includes: preparing a heavy metal colloid solution, adding an adhesive, adhering to the heavy metal colloid solution, making a composite film laminate, cutting and encapsulating; five major steps, firstly preparing a heavy metal colloid by heavy metal salt , And then add a heating and volatile adhesive to the heavy metal colloid to increase the viscosity of the heavy metal colloid, and then pass the light metal film through the viscous heavy metal colloid to obtain two adhesive light metal films that adhere to the heavy metal layer, and then combine the light metal film and the adhesive The flexible light metal film is folded alternately to obtain a composite film stack, and finally the composite film stack is cut and encapsulated to obtain a grating 7. The whole production process of the present invention is short, the cost price is low, and the production process is convenient and quick. The fabricated structure will not collapse. By controlling the width of the light element metal sheet, it can be used to fabricate gratings of any area. Through one fabrication, X-ray gratings can be mass-produced.
附图说明Description of the drawings
图1为本发明的工艺流程图;Figure 1 is a process flow diagram of the present invention;
图2为直接采购的金属膜滚筒结构示意图;Figure 2 is a schematic diagram of the directly purchased metal film drum structure;
图3为本发明的轻金属膜通过经过物理滚压技术得到预定厚度示意图;3 is a schematic diagram of the light metal film of the present invention obtained by physical rolling technology to obtain a predetermined thickness;
图4为本发明的轻金属膜形成粘性轻金属膜1的示意图;4 is a schematic diagram of the light metal film of the present invention forming a viscous light metal film 1;
图5为本发明的粘性轻金属膜与轻金属模块堆叠第一步骤示意图;5 is a schematic diagram of the first step of stacking the adhesive light metal film and the light metal module of the present invention;
图6为本发明的粘性轻金属膜与轻金属模块堆叠第二步骤示意图;6 is a schematic diagram of the second step of stacking the adhesive light metal film and the light metal module of the present invention;
图7为本发明的粘性轻金属膜与轻金属模块堆叠第三步骤示意图;7 is a schematic diagram of the third step of stacking the adhesive light metal film and the light metal module of the present invention;
图8为本发明的粘性轻金属膜块与轻金属模块堆示意图;FIG. 8 is a schematic diagram of the sticky light metal film block and the light metal module stack of the present invention;
图9为本发明的粘性轻金属膜与轻金属模垂直卷叠示意图;FIG. 9 is a schematic view of the sticky light metal film and the light metal mold being vertically rolled and stacked according to the present invention;
图10为本发明的粘性轻金属膜卷叠示意图;FIG. 10 is a schematic diagram of the roll of the viscous light metal film of the present invention;
图11为本发明的切割第一形状复合膜堆4得到准光栅5示意图;11 is a schematic diagram of the quasi-grating 5 obtained by cutting the first shape composite film stack 4 of the present invention;
图12为本发明的切割第一形状复合膜堆4示意图;FIG. 12 is a schematic diagram of the first-shaped composite membrane stack 4 according to the present invention;
图13为本发明的准光栅结构示意图;Figure 13 is a schematic diagram of the quasi-grating structure of the present invention;
图14为本发明的光栅结构示意意图。Fig. 14 is a schematic diagram of the grating structure of the present invention.
主要元件符号说明如下:The main component symbols are explained as follows:
1、轻金属膜;2、重金属层;11、滚轮;13、连接部;4、第一形状复合膜堆;5、准光栅;6、碳素纤维;7、光栅。1. Light metal film; 2. Heavy metal layer; 11. Roller; 13. Connection part; 4. First shape composite film stack; 5. Quasi-grating; 6. Carbon fiber; 7. Grating.
本发明的实施方式Embodiments of the present invention
为了更清楚地表述本发明,下面结合附图对本发明作进一步地描述。In order to express the present invention more clearly, the present invention will be further described below with reference to the accompanying drawings.
光在衍射过程中满足公式(a+b)(sinφ+sinθ)=k λ;其中,式中a代表狭缝宽度,b代表狭缝间距,φ为衍射角,θ为光的入射方向与光栅7平面法线之间的夹角,k为明条纹光谱级数(k=0,±1,±2……),λ为波长,a+b称作光栅7常数;光栅7产生的条纹的特点是:明条纹很亮很窄,相邻明纹间的暗区很宽,衍射图样十分清晰;如果由于制作误差导致狭缝宽度和狭缝间距值偏差过大,会导致在衍射时成像模糊,最终通过X射线得到的图像就会是一片模糊、分辨不清的;特别在医疗应用中,图像不清容易导致疾病检查的误差率非常高;因此如何批量精准生产光栅7成为目前极具市场前景的技术点。In the diffraction process, the light satisfies the formula (a+b)(sinφ+sinθ)=k λ; where a represents the slit width, b represents the slit spacing, φ is the diffraction angle, and θ is the incident direction of the light and the grating 7 The angle between the normals of the plane, k is the number of bright fringe spectrum (k=0, ±1, ±2...), λ is the wavelength, and a+b is called the grating 7 constant; the fringe produced by the grating 7 The characteristics are: bright stripes are very bright and narrow, the dark area between adjacent bright stripes is very wide, and the diffraction pattern is very clear; if the deviation of the slit width and the slit spacing is too large due to manufacturing errors, the image will be blurred during diffraction , The final image obtained by X-rays will be blurred and unclear; especially in medical applications, unclear images can easily lead to a very high error rate in disease inspection; therefore, how to accurately produce grating 7 in batches has become a market today. Prospect of technical points.
正如背景技术所说,目前制作光栅7的工艺主要是包括DRIE技术、LIGA技术和硅基光助电化学刻蚀技术;DRIE技术制作光栅7的过程中X光源需要昂贵的加速器,成本高,且用于X光光刻的掩膜板本身就是3D微观结构,制作周期长; LIGA技术在制作光栅7时经常有光栅7断裂坍塌等引起结构失效的现象发生。且制作成本较高,可制作面积较小;光助电化学刻蚀方法则流程复杂,而且制作过程中硅基电阻率、温度、腐蚀液等均对刻蚀结构的影响较大,难以控制,在后期的高原子序数金属填充过程中,所需的填充工艺复杂,条件也较为苛刻;目前尚未出现一种成本低,周期短,制作方便,且适合大批量生产的光栅7制作工艺。As mentioned in the background art, the current process for making grating 7 mainly includes DRIE technology, LIGA technology and silicon-based photo-assisted electrochemical etching technology; in the process of making grating 7 by DRIE technology, the X light source requires expensive accelerators, and the cost is high. The mask used for X-ray lithography is itself a 3D microstructure with a long production cycle; in the LIGA technology, when the grating 7 is produced, the grating 7 often breaks and collapses and causes structural failure. In addition, the production cost is relatively high, and the production area is small; the photo-assisted electrochemical etching method has a complicated process, and the silicon-based resistivity, temperature, and etching solution during the production process have a large impact on the etching structure, which is difficult to control. In the later high atomic number metal filling process, the required filling process is complicated and the conditions are relatively harsh; currently, there has not yet been a low cost, short cycle, convenient manufacturing process and suitable for mass production of the grating 7 manufacturing process.
基于此,本申请提供了一种轻金属膜1粘附重金属胶体的光栅7制作工艺,请参阅图1,其包括以下步骤:Based on this, the present application provides a manufacturing process for grating 7 with light metal film 1 adhered to heavy metal colloid. Please refer to FIG. 1, which includes the following steps:
制备重金属胶体溶液:向重金属盐溶液中依次添加分散剂和还原剂得到分散的胶体溶液;Prepare heavy metal colloidal solution: add dispersant and reducing agent to heavy metal salt solution in order to obtain dispersed colloidal solution;
添加粘合剂:在制备好的重金属胶体溶液里加入粘合剂得到粘性重金属胶体溶液;Add adhesive: add adhesive to the prepared heavy metal colloid solution to obtain a viscous heavy metal colloid solution;
粘附重金属胶体溶液:将轻金属膜1传送至粘性重金属胶体溶液中,使得重金属颗粒粘附在轻元素金属板上后再将轻金属膜1传送出,得到粘附性轻金属膜1;Adhesive heavy metal colloid solution: transfer the light metal film 1 to the viscous heavy metal colloid solution, so that the heavy metal particles adhere to the light element metal plate and then transfer the light metal film 1 out to obtain the adhesive light metal film 1;
制作复合膜叠层:将轻金属膜1和粘附性轻金属膜1相互叠合,得到复合膜叠层;Making a composite film stack: stack the light metal film 1 and the adhesive light metal film 1 on each other to obtain a composite film stack;
切割:按设定尺寸切割后的复合膜堆,得到准光栅5;Cutting: The composite film stack is cut according to the set size to obtain the quasi-grating 5;
封装:使用X射线弱吸收材料封装准光栅5得到光栅7。Packaging: The quasi-grating 5 is packaged with a weak X-ray absorbing material to obtain the grating 7.
在本工艺流程中,共包括制备重金属胶体溶液、添加粘合剂、粘附重金属胶体溶液、制作复合膜叠层、切割和封装,五大步骤,整个本发明制作光栅7制作周期短,成本价格低,制作过程方便快捷;制作的结构不会垮塌,通过控制轻元素金属板材的宽度,用来制作任意面积的光栅7,通过一次制作,可大批量生产出X射线光栅7。In this process, there are five steps including preparation of heavy metal colloid solution, addition of adhesive, adhesion of heavy metal colloid solution, production of composite film lamination, cutting and packaging. The entire production cycle of the grating 7 of the present invention is short and the cost is low. The production process is convenient and quick; the produced structure will not collapse. By controlling the width of the light element metal sheet, it can be used to produce gratings 7 of any area. Through one production, X-ray gratings 7 can be mass-produced.
请参阅图2,制备重金属胶体溶液时,先向重金属盐溶液中加入浓氨水得到重金属氨络合物溶液,再向重金属氨络合物溶液中加入分散剂,并搅拌均匀后,逐滴滴加还原剂,搅拌均匀后得到纳米级重金属胶体。Please refer to Figure 2. When preparing the heavy metal colloidal solution, first add concentrated ammonia to the heavy metal salt solution to obtain the heavy metal ammonia complex solution, and then add the dispersant to the heavy metal ammonia complex solution, and stir evenly, then add dropwise Reducing agent, after stirring evenly, a nano-scale heavy metal colloid is obtained.
在本实施例中,重金属可以为钨,银,铅,金等原子序数大的金属;对应的重金属盐溶液包括醋酸铅溶液、硝酸盐溶液、三氯化金溶液等;该溶液可以直接从市面购买相应的粉末,直接溶于水即可得到;得到金属盐溶液后,先向金属盐溶液中加入浓氨水,得到金属氨络合物溶液;其中浓氨水中铵离子的浓度大于15%;分散剂包括碱金属磷酸盐类,例如:三聚磷酸钠、六偏磷酸钠和焦磷酸钠、月桂酸、三乙基己基磷酸、十二烷基硫酸钠、甲基戊醇、纤维素衍生物、聚丙烯酰胺、古尔胶、脂肪酸聚乙二醇酯等;加入分散剂后使得络合物溶解;待络合物溶解后,加入还原剂,还原得到重金属胶体;常见的还原剂包括硫化氢、碘化钾、金属单质、氢气、一氧化碳气体、硼氢化钠等;搅拌均匀后可以通过丁达尔效应测试反应结果。在本实施例中,搅拌均匀后,可以继续通过超声波仪器使纳米级重金属颗粒均匀分散在胶体溶液中。In this embodiment, the heavy metals can be metals with large atomic numbers such as tungsten, silver, lead, gold; the corresponding heavy metal salt solutions include lead acetate solution, nitrate solution, gold trichloride solution, etc.; the solution can be purchased directly from the market The corresponding powder can be obtained by directly dissolving in water; after obtaining the metal salt solution, first add concentrated ammonia water to the metal salt solution to obtain a metal ammonia complex solution; wherein the concentration of ammonium ions in the concentrated ammonia water is greater than 15%; dispersant Including alkali metal phosphates, such as: sodium tripolyphosphate, sodium hexametaphosphate and sodium pyrophosphate, lauric acid, triethylhexyl phosphoric acid, sodium lauryl sulfate, methylpentanol, cellulose derivatives, poly Acrylamide, Guer gum, fatty acid polyethylene glycol ester, etc.; dissolve the complex after adding dispersant; after the complex is dissolved, add a reducing agent to reduce to obtain heavy metal colloids; common reducing agents include hydrogen sulfide and potassium iodide , Metal element, hydrogen, carbon monoxide gas, sodium borohydride, etc.; after stirring evenly, the reaction result can be tested by the Tyndall effect. In this embodiment, after the stirring is uniform, the ultrasonic instrument can be used to uniformly disperse the nano-scale heavy metal particles in the colloidal solution.
在本实施例中,制备重金属胶体溶液时,重金属盐与分散剂的摩尔比为11:1—12:1,优选的为11.6:1。In this embodiment, when preparing the heavy metal colloidal solution, the molar ratio of the heavy metal salt to the dispersant is 11:1-12:1, preferably 11.6:1.
在本实施例中,制备滴加还原剂时,重金属盐与还原剂的摩尔比为3:1—5:1;优选的为4:1。In this embodiment, when preparing the dropping reducing agent, the molar ratio of the heavy metal salt to the reducing agent is 3:1-5:1; preferably 4:1.
实施例1:Example 1:
将30g 硝酸银溶于150 mL 蒸馏水和30mL 浓氨水中,配制成银氨络合物溶液; 再将7.5g月桂酸溶于1000mL 蒸馏水和75 mL 浓氨水中,配制成月桂酸水溶液;开启电动搅拌装置将银氨溶液与月桂酸水溶液混合均匀,控制搅拌速度在 800 ~ 1000 r /min。常温下,向上述混合溶液逐滴滴加 NaBH4 溶液,还原剂 NaBH4 与硝酸银的摩尔比为[AgNO3] /[NaBH4]= 4,滴加完成后再搅拌 1 h,即可得到黑色的纳米银胶体;当需要制备大量的纳米银胶体时,可以通过等比例增加试剂量即可。Dissolve 30g of silver nitrate in 150mL of distilled water and 30mL of concentrated ammonia to prepare a silver ammonia complex solution; then dissolve 7.5g of lauric acid in 1000mL of distilled water and 75mL of concentrated ammonia to prepare an aqueous solution of lauric acid; turn on electric stirring The device mixes the silver ammonia solution and the lauric acid aqueous solution uniformly, and controls the stirring speed at 800-1000 r/min. At room temperature, add dropwise to the above mixed solution NaBH4 solution, the molar ratio of reducing agent NaBH4 to silver nitrate is [AgNO3] /[NaBH4] = 4. After the addition is complete, stir for 1 h to obtain black nano silver colloid; when a large amount of nano silver colloid needs to be prepared , You can increase the amount of reagents in equal proportions.
在本实施例中,添加粘合剂时,粘合剂为加热易挥发形粘合剂;粘合剂包括双酚A型,线型甲酚型,酚醛环氧树脂、聚氨酯胶粘剂等;优选的采用:基丙烯酸乙酯做粘合剂。In this embodiment, when the adhesive is added, the adhesive is a heat-volatile adhesive; the adhesive includes bisphenol A type, novolac type, novolac epoxy resin, polyurethane adhesive, etc.; preferably Adopt: ethyl acrylate as adhesive.
请参阅图4,制作粘性轻金属膜1时,轻金属膜1两面均粘附重金属层2;通过控制重金属胶体的颗粒浓度控制重金属层2的厚度。Referring to FIG. 4, when the viscous light metal film 1 is made, the heavy metal layer 2 is adhered to both sides of the light metal film 1; the thickness of the heavy metal layer 2 is controlled by controlling the particle concentration of the heavy metal colloid.
在本实施例中,轻金属材料为铝或铍等原子序数小的金属;通常预制好的轻金属膜1的厚度为50-80微米;宽度约为5-10厘米;像卷纸一样卷绕在滚筒上;轻金属膜1是通过拉压工艺制成,在市面上有成品直接销售;轻金属膜1是预制好的,将轻金属膜1制作与光栅7制作分离开,为每种工艺流程提供独立的环境,更有利于流水线大批量生产;且轻金属膜1能够预先设定好尺寸,更好地控制精度,使其在光栅7制作中误差较小。In this embodiment, the light metal material is a metal with a small atomic number such as aluminum or beryllium; usually the prefabricated light metal film 1 has a thickness of 50-80 microns; a width of about 5-10 cm; it is wound on a roller like a roll of paper Above; the light metal film 1 is made through a drawing and pressing process, and there are finished products on the market for direct sale; the light metal film 1 is prefabricated, and the production of the light metal film 1 is separated from the production of the grating 7 to provide an independent environment for each process , It is more conducive to mass production of the assembly line; and the size of the light metal film 1 can be preset to better control the accuracy, so that the error in the production of the grating 7 is smaller.
在本实施例中,轻金属膜1在传输至重金属胶体溶液之前,先从滚筒上被拉出,拉出后以运输通过滚压设备,滚压设备将轻金属膜1的厚度滚压至设定值;例如设定值为30微米,轻金属膜1的厚度从原60微米被滚压至30微米,轻金属膜1被滚压后继续被传送至重金属胶体池中,通过胶体池后再被传送出,轻金属膜1两面均粘附有重金属粒子层,形成粘附性轻金属膜1;其中,重金属层2的厚度由胶体的颗粒溶度决定;例如,重金属胶体的溶度为15.2g/L,轻金属膜1通过重金属胶体的时间为1min,轻金属膜1两面均形成厚度为25微米的重金属层2。In this embodiment, the light metal film 1 is pulled out of the roller before being transferred to the heavy metal colloid solution, and after being pulled out, it is transported through the rolling equipment, and the rolling equipment rolls the thickness of the light metal film 1 to the set value. ; For example, the setting value is 30 microns, and the thickness of the light metal film 1 is rolled from 60 microns to 30 microns. After the light metal film 1 is rolled, it continues to be transported to the heavy metal colloid pool, and then is transported out after passing through the colloid pool. The light metal film 1 has heavy metal particle layers adhered on both sides to form an adhesive light metal film 1. The thickness of the heavy metal layer 2 is determined by the particle solubility of the colloid; for example, the solubility of the heavy metal colloid is 15.2g/L, and the light metal film 1 The time to pass through the heavy metal colloid is 1 min, and the heavy metal layer 2 with a thickness of 25 microns is formed on both sides of the light metal film 1.
在本实施例中,轻金属膜1从滚筒上拉出到滚压再到传送至粘性重金属胶体溶液并传出,整个过程中轻金属膜1可以是始终未被拉断的长条形,也可以是先将轻金属膜1从滚筒上拉断后,再依次经过滚压设备和粘性重金属胶体;例如轻金属膜1从滚筒上拉出后,被切割成长10cm,宽5cm,厚60微米的轻金属膜1块,再通过滚轮11,并依次经形后续的加工。In this embodiment, the light metal film 1 is drawn from the roller, rolled, and then transferred to the viscous heavy metal colloid solution and passed out. In the whole process, the light metal film 1 can be a long strip that has not been broken, or it can be First pull off the light metal film 1 from the drum, and then pass through the rolling equipment and viscous heavy metal colloid in sequence; for example, after the light metal film 1 is pulled from the drum, it is cut into a piece of light metal film with a length of 10 cm, a width of 5 cm and a thickness of 60 microns. Then pass the roller 11, and follow-up processing in turn.
在本实施例中,还可以通过直接向轻金属膜1上喷射重金属胶体的方式得到粘性轻金属膜1;轻金属先从滚筒上被拉出后通过滚压设备,滚压设备将轻金属膜1的厚度滚压至设定值;再直接往轻金属膜1上双面喷射重金属胶体。In this embodiment, the viscous light metal film 1 can also be obtained by directly spraying heavy metal colloid on the light metal film 1. The light metal is first pulled out of the roller and then passed through a rolling device, which rolls the thickness of the light metal film 1 Press to the set value; then directly spray heavy metal colloid on both sides of the light metal film 1.
在本实施例中,粘附重金属胶体溶液后,还需要对粘附性轻金属膜1进行加热处理,使其粘合剂液体挥发,重金属颗粒固化在轻元素金属表面上最终得到粘性轻金属膜1, 粘合剂液体挥过程中重金属层2的厚度不发生变化;从粘性重金属胶体中传输出来后通过恒温加热装置,使其粘合剂液体挥发,重元素金属颗粒固化在轻元素金属表面上,恒温温度和加热时间视加入的粘合剂的种类不同而不同;例如:粘合剂为基丙烯酸乙酯做粘合剂,加热时间为10min,加热温度为80度, 粘合剂液体挥发完全,加热前重金属层2的厚度为25微米,加热后重金属层2的厚度仍为25微米。In this embodiment, after the heavy metal colloidal solution is adhered, the adhesive light metal film 1 needs to be heated to volatilize the adhesive liquid, and the heavy metal particles are solidified on the light element metal surface to finally obtain the adhesive light metal film 1. The thickness of the heavy metal layer 2 does not change during the volatilization of the adhesive liquid; after being transferred from the viscous heavy metal colloid, the adhesive liquid is volatilized by a constant temperature heating device, and the heavy element metal particles are solidified on the light element metal surface at a constant temperature. The temperature and heating time are different depending on the type of adhesive added; for example: the adhesive is ethyl acrylate as the adhesive, the heating time is 10min, the heating temperature is 80 degrees, the adhesive liquid is completely volatilized, heating The thickness of the front heavy metal layer 2 is 25 microns, and the thickness of the heavy metal layer 2 is still 25 microns after heating.
请参阅图5,制作复合膜叠层时,轻金属膜1和粘性轻金属膜1交错折叠,形成轻金属膜1重金属层2间隔堆叠的复合膜堆,单层轻金属膜1的厚度D与其表面的重金属膜层厚度d之和为光栅7的周期n。Please refer to Figure 5, when the composite film laminate is made, the light metal film 1 and the viscous light metal film 1 are folded alternately to form a composite film stack in which the light metal film 1 and the heavy metal layer 2 are stacked at intervals. The thickness D of the single light metal film 1 and the heavy metal film on its surface The sum of the layer thickness d is the period n of the grating 7.
实施例2:Example 2:
粘性轻金属膜1为未被拉断的长条形,轻金属膜1预先被切割成设定的形状大小的轻金属膜1块,例如长度为10cm,宽度为6cm,厚度为30微米的轻金属模块;粘性轻金属的宽度为6cm,厚度为30微米,粘性轻金属上的重金属层2厚度为50微米;以轻金属膜1为底层,在轻金属膜1上覆盖一层粘性轻金属膜1,再在粘性轻金属膜1上堆叠轻金属膜1,交替堆叠形成符合膜堆,光栅7周期为80微米;其中,交替堆叠是采用Z字形堆叠法,堆叠效率高;该复合膜堆的相对两侧面会产生因为粘性金属膜弯卷产生的连接部13。The viscous light metal film 1 is a long strip that has not been broken. The light metal film 1 is pre-cut into a light metal film of a predetermined shape and size, such as a light metal module with a length of 10 cm, a width of 6 cm, and a thickness of 30 microns; The width of the light metal is 6cm, the thickness is 30 microns, and the thickness of the heavy metal layer 2 on the viscous light metal is 50 microns; with the light metal film 1 as the bottom layer, a layer of viscous light metal film 1 is covered on the light metal film 1, and then on the viscous light metal film 1. Stack the light metal film 1, alternately stacked to form a conforming film stack, the grating 7 period is 80 microns; among them, the alternate stacking adopts the zigzag stacking method, which has high stacking efficiency; the two opposite sides of the composite film stack will be curled due to the viscous metal film The resulting connection portion 13.
实施例3:Example 3:
轻金属膜1和粘性轻金属膜1均被拉断成设定大小的金属膜块,轻金属膜1块通过滚压设备后被切割成设定的形状大小的轻金属膜1块,例如切割成长度为10cm,宽度为6cm,厚度为30微米的粘性轻金属模块,粘性轻金属上的重金属层2厚度为50微米;轻金属膜1的尺寸与粘性轻金属的尺寸完全相同;直接将轻金属膜1块和粘性金属模块正交交错堆叠,形成复合膜堆;光栅7周期为80微米。Both the light metal film 1 and the viscous light metal film 1 are pulled into pieces of metal film of a set size, and one piece of light metal film is cut into a piece of light metal film of a set shape and size after passing through the rolling equipment, for example, cut into a length of 10cm , A viscous light metal module with a width of 6cm and a thickness of 30 microns. The thickness of the heavy metal layer 2 on the viscous light metal is 50 microns; the size of the light metal film 1 is exactly the same as the size of the viscous light metal; the light metal film 1 is directly connected to the viscous metal module. Interleaved stacked to form a composite film stack; the grating 7 has a period of 80 microns.
实施例4:Example 4:
轻金属膜1和粘性轻金属膜1均为未被拉断的长条形,制作复合膜叠层时,轻金属和粘性轻金属尺寸均为宽度6cm,厚度30微米,重金属层2厚度50微米;将轻金属膜1至第一方向放置,粘性金属膜至第二方向放置,第一方向和第二方向相互垂直;交错折叠轻金属膜1和粘性轻金属膜1,形成长度和宽度均为6cm的复合膜堆;光栅7周期为80微米;且光栅7相邻面会产生因为粘性金属膜和轻金属膜1弯卷产生的连接部13。The light metal film 1 and the viscous light metal film 1 are both long and unbroken. When the composite film is made, the size of the light metal and the viscous light metal are both 6cm in width and 30 microns in thickness, and the thickness of the heavy metal layer 2 is 50 microns; 1. Place the adhesive metal film in the first direction, place the adhesive metal film in the second direction, the first direction and the second direction are perpendicular to each other; interfold the light metal film 1 and the adhesive light metal film 1 to form a composite film stack with a length and a width of 6 cm; The 7 period is 80 micrometers; and the adjacent surface of the grating 7 will have a connection portion 13 due to the bending of the viscous metal film and the light metal film 1.
请参阅图6,制作复合膜叠层时,可以直接卷叠粘性轻金属膜1,形成轻金属膜1和重金属层2间隔堆叠的复合膜堆,粘性轻金属膜1的厚度为D,重金属层2厚度为d,光栅7周期n=D+2*n。Please refer to Figure 6, when making a composite film laminate, you can directly roll the viscous light metal film 1 to form a composite film stack in which the light metal film 1 and the heavy metal layer 2 are stacked at intervals. The thickness of the viscous light metal film 1 is D, and the thickness of the heavy metal layer 2 is d, the grating 7 period n=D+2*n.
实施例5:Example 5:
粘性轻金属膜1为未被拉断的长条形,制作复合膜叠层时,粘性轻金属膜1尺寸为宽度6cm,厚度30微米,重金属层2厚度50微米;直接将长条形粘性金属膜按照设定的长度,往复折叠即可得到轻金属膜1和重金属层2交错排列的复合膜堆,其复合膜堆中光栅7的周期为130微米;复合膜堆的相对面会产生因为粘性金属膜和轻金属膜1弯卷产生的连接部13。The viscous light metal film 1 is a long strip that is not broken. When making a composite film laminate, the size of the viscous light metal film 1 is 6cm in width, 30 microns in thickness, and the heavy metal layer 2 is 50 microns in thickness; Set the length and fold back and forth to obtain a composite membrane stack with light metal film 1 and heavy metal layer 2 staggered. The period of the grating 7 in the composite membrane stack is 130 microns; The connecting portion 13 produced by the bending of the film 1.
请参阅图7,得到复合膜堆后,对符合膜堆进行切割;切割复合膜堆时,先切割复合膜堆的边缘得到第一形状的复合膜堆,再按设定尺寸切割第一形状的复合膜堆,得到准光栅5;由于在制作复合膜的过程中,复合膜堆存在连接部13或者金属膜无法做到完全边与边对准,所以需要先对符合膜的边进行切除,只保留完全重合的中间部分,其中切除的位置为复合膜堆的边缘大于1cm处;优选的切除后的复合膜堆为长方体形;切除时采用激光切除或者线切割机、或者铣刀;优选的采用大功率激光切割,切割时精度可达到0.01mm。Please refer to Figure 7, after obtaining the composite membrane stack, cut the conforming membrane stack; when cutting the composite membrane stack, first cut the edge of the composite membrane stack to obtain the composite membrane stack of the first shape, and then cut the first shape according to the set size The composite film stack is used to obtain the quasi-grating 5; since the composite film stack has the connecting part 13 or the metal film cannot be completely aligned with the edge during the process of making the composite film, it is necessary to cut off the edge that conforms to the film first. Keep the completely overlapped middle part, where the cut position is where the edge of the composite membrane stack is greater than 1cm; the composite membrane stack after removal is preferably a rectangular parallelepiped; laser resection or wire cutting machine or milling cutter is used for resection; preferably High-power laser cutting, the precision can reach 0.01mm during cutting.
在本实施例中,第一形状可以为多边形、矩形、三角形或者其他形状;优选的第一形状为矩形。In this embodiment, the first shape may be a polygon, a rectangle, a triangle or other shapes; the preferred first shape is a rectangle.
请参阅图8-图14,得到第一形状复合膜堆4后,沿着复合膜堆的宽度方向切割第一形状得到多条准光栅5,以第一形状的厚度方向为准光栅5的宽度,第一形状的宽度方向为准光栅5的长度方向;切割间距为为准光栅5的厚度方向;切割后的得到的光栅7的长度一致;整个切割过程中,光栅7的厚度方向无需切割,且仅切割次数少,制作精度高。Referring to Figures 8-14, after obtaining the composite film stack 4 of the first shape, the first shape is cut along the width direction of the composite film stack to obtain a plurality of quasi gratings 5, and the thickness direction of the first shape is the width of the quasi grating 5 , The width direction of the first shape is the length direction of the quasi grating 5; the cutting pitch is the thickness direction of the quasi grating 5; the length of the grating 7 obtained after cutting is the same; the thickness direction of the grating 7 does not need to be cut during the entire cutting process, And only the number of cuts is small, and the production precision is high.
在本实施例中,切割第一形状是时,切割方向和角度可任意调整,切割后,并不限于垂直切割。In this embodiment, when cutting the first shape, the cutting direction and angle can be adjusted arbitrarily, and after cutting, it is not limited to vertical cutting.
请参阅图9,在封装过程中,利用碳素纤维6材料膜夹持第一形状宽度方向的切割面,直至碳素纤维6黏合各层复合膜,完成封装,得到光栅7。Please refer to FIG. 9, in the packaging process, the carbon fiber 6 material film is used to clamp the cut surface in the width direction of the first shape until the carbon fiber 6 adheres to the composite film of each layer to complete the packaging, and the grating 7 is obtained.
 To
工业实用性Industrial applicability
本发明的优势在于:The advantages of the present invention are:
1、可以利用物理滚压技术将轻金属膜1压缩至预定厚度为D后,再将轻金属膜1通过重金属胶体,得到设定尺寸的粘性轻金属膜1;1. The light metal film 1 can be compressed to a predetermined thickness D by physical rolling technology, and then the light metal film 1 can be passed through a heavy metal colloid to obtain a viscous light metal film 1 of a set size;
2、本发明制作光栅7制作周期短,成本价格低,制作过程方便快捷;制作的结构不会垮塌,通过控制轻元素金属板材的宽度,用来制作任意面积的光栅7。通过一次制作,可大批量生产出X射线光栅7。2. The production cycle of the grating 7 produced by the present invention is short, the cost is low, and the production process is convenient and quick; the produced structure will not collapse, and the grating 7 of any area can be produced by controlling the width of the light element metal plate. Through one production, X-ray grating 7 can be produced in large quantities.
   3、轻金属膜1在制作成复合膜堆之前可以不进行裁剪正常加工,堆叠形成复合膜堆后再切割。To 3. Before the light metal film 1 is made into a composite film stack, normal processing may not be performed, and the composite film stack can be stacked to form a composite film stack and then cut.
序列表自由内容Sequence Listing Free Content
以上公开的仅为本发明的几个具体实施例,但是本发明并非局限于此,任何本领域的技术人员能思之的变化都应落入本发明的保护范围。The above disclosures are only a few specific embodiments of the present invention, but the present invention is not limited thereto, and any changes that can be thought of by those skilled in the art should fall into the protection scope of the present invention.

Claims (10)

  1. 一种轻金属膜粘附重金属胶体的光栅制作工艺,其特征在于,包括A grating manufacturing process with light metal film adhered to heavy metal colloid, which is characterized in that it comprises
    制备重金属胶体溶液:向重金属盐溶液中依次添加分散剂和还原剂得到重金属胶体溶液;Preparation of heavy metal colloid solution: adding dispersant and reducing agent to heavy metal salt solution in order to obtain heavy metal colloid solution;
    添加粘合剂:在制备好的重金属胶体溶液里加入粘合剂得到粘性重金属胶体溶液;Add adhesive: add adhesive to the prepared heavy metal colloid solution to obtain a viscous heavy metal colloid solution;
    制作粘性轻金属膜:将轻金属膜传送至粘性重金属胶体溶液中,使得重金属颗粒粘附在轻元素金属板上后再将轻金属膜传送出,得到粘性轻金属膜;Making a viscous light metal film: transfer the light metal film to a viscous heavy metal colloid solution, so that the heavy metal particles adhere to the light element metal plate, and then the light metal film is transported out to obtain a viscous light metal film;
    制作复合膜叠层:将轻金属膜和粘性轻金属膜相互叠合,得到复合膜叠层;Making a composite film stack: stack the light metal film and the viscous light metal film with each other to obtain a composite film stack;
    切割:按设定尺寸切割后的复合膜堆,得到准光栅;Cutting: The composite film stack is cut according to the set size to obtain the quasi-grating;
    封装:使用X射线弱吸收材料封装准光栅得到光栅。Packaging: Use the X-ray weak absorption material to package the quasi-grating to obtain the grating.
  2. 根据权利要求1所述的轻金属膜粘附重金属胶体的光栅制作工艺,其特征在于,制备重金属胶体溶液时,先向重金属盐溶液中加入浓氨水得到金属氨络合物溶液,再向金属氨络合物溶液中加入分散剂,并搅拌均匀后,逐滴滴加还原剂,搅拌均匀后得到纳米级重金属胶体。The grating manufacturing process of light metal film adhering heavy metal colloid according to claim 1, wherein when preparing the heavy metal colloid solution, first add concentrated ammonia water to the heavy metal salt solution to obtain the metal ammonia complex solution, and then add the metal ammonia complex solution to the heavy metal salt solution. Add a dispersant to the compound solution and stir it evenly, then add the reducing agent drop by drop, and stir evenly to obtain a nano-scale heavy metal colloid.
  3. 据权利要求2所述的轻金属膜粘附重金属胶体的光栅制作工艺,其特征在于,制备重金属胶体溶液时,重金属盐与分散剂的摩尔比为11:1—12:1。The grating manufacturing process of light metal film adhered to heavy metal colloid according to claim 2, characterized in that, when preparing the heavy metal colloid solution, the molar ratio of the heavy metal salt to the dispersant is 11:1-12:1.
  4. 据权利要求2所述的轻金属膜粘附重金属胶体的光栅制作工艺,其特征在于,制备滴加还原剂时,重金属盐与还原剂的摩尔比为3:1—5:1。The grating manufacturing process for light metal film adhered to heavy metal colloid according to claim 2, characterized in that when preparing the dropwise reducing agent, the molar ratio of the heavy metal salt to the reducing agent is 3:1-5:1.
  5. 据权利要求1所述的轻金属膜粘附重金属胶体的光栅制作工艺,其特征在于,添加粘合剂时,粘合剂为加热易挥发形粘合剂。The grating manufacturing process of light metal film adhering heavy metal colloid according to claim 1, characterized in that when the adhesive is added, the adhesive is a heated and volatile adhesive.
  6. 据权利要求1所述的轻金属膜粘附重金属胶体的光栅制作工艺,其特征在于,制作粘性轻金属膜时,轻金属膜两面均粘附重金属层;通过控制重金属胶体溶液的浓度控制重金属层的厚度。The grating manufacturing process for light metal film adhered to heavy metal colloid according to claim 1, characterized in that when the viscous light metal film is made, the heavy metal layer is adhered to both sides of the light metal film; the thickness of the heavy metal layer is controlled by controlling the concentration of the heavy metal colloid solution.
  7. 据权利要求6所述的轻金属膜粘附重金属胶体的光栅制作工艺,其特征在于,制作粘性轻金属膜时,需要对两面均粘附重金属层的轻金属膜进行加热处理,使其粘合剂液体挥发,重金属颗粒固化在轻元素金属表面上。The grating manufacturing process with light metal film adhered to heavy metal colloid according to claim 6, characterized in that, when making the viscous light metal film, it is necessary to heat the light metal film with the heavy metal layer adhered on both sides to make the adhesive liquid volatilize , The heavy metal particles are solidified on the surface of the light element metal.
  8. 据权利要求1所述的轻金属膜粘附重金属胶体的光栅制作工艺,其特征在于,制作复合膜叠层时,将粘性轻金属膜和轻金属膜交错折叠或者直接卷叠粘性轻金属膜,形成轻金属膜和重金属层间隔堆叠的复合膜堆。The grating manufacturing process of light metal film adhered to heavy metal colloid according to claim 1, characterized in that, when making the composite film laminate, the viscous light metal film and the light metal film are alternately folded or the viscous light metal film is directly rolled to form the light metal film and A composite membrane stack in which heavy metal layers are stacked at intervals.
  9. 根据权利要求1所述的轻金属膜粘附重金属胶体的光栅制作工艺,其特征在于,切割复合膜堆时,先切割复合膜堆的边缘得到第一形状的复合膜堆,再按设定尺寸切割第一形状的复合膜堆,得到准光栅。The grating manufacturing process of light metal film adhering heavy metal colloid according to claim 1, wherein when cutting the composite film stack, the edge of the composite film stack is first cut to obtain the composite film stack of the first shape, and then the composite film stack is cut according to the set size. The composite membrane stack of the first shape obtains the quasi-grating.
  10. 根据权利要求1所述的轻金属膜粘附重金属胶体的光栅制作工艺,其特征在于,在封装过程中,利用碳素纤维材料板夹持准光栅的切割面,直至碳素纤维黏合各复合膜,完成封装。The grating manufacturing process of light metal film adhering heavy metal colloid according to claim 1, characterized in that, in the packaging process, the cut surface of the quasi grating is clamped by the carbon fiber material plate until the carbon fiber is bonded to each composite film. Complete the package.
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