CN113782416B - Tellurium-cadmium-mercury liquid phase epitaxial growth source substrate and preparation method thereof, and tellurium-cadmium-mercury liquid phase epitaxial growth method - Google Patents

Tellurium-cadmium-mercury liquid phase epitaxial growth source substrate and preparation method thereof, and tellurium-cadmium-mercury liquid phase epitaxial growth method Download PDF

Info

Publication number
CN113782416B
CN113782416B CN202111070423.7A CN202111070423A CN113782416B CN 113782416 B CN113782416 B CN 113782416B CN 202111070423 A CN202111070423 A CN 202111070423A CN 113782416 B CN113782416 B CN 113782416B
Authority
CN
China
Prior art keywords
cadmium
tellurium
mercury
substrate
plating layer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202111070423.7A
Other languages
Chinese (zh)
Other versions
CN113782416A (en
Inventor
许军
杨晓杰
龚月
李承林
李想
赵倩
毛成状
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui Guangzhi Technology Co Ltd
Original Assignee
Anhui Guangzhi Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Anhui Guangzhi Technology Co Ltd filed Critical Anhui Guangzhi Technology Co Ltd
Priority to CN202111070423.7A priority Critical patent/CN113782416B/en
Publication of CN113782416A publication Critical patent/CN113782416A/en
Application granted granted Critical
Publication of CN113782416B publication Critical patent/CN113782416B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02518Deposited layers
    • H01L21/02521Materials
    • H01L21/02551Group 12/16 materials
    • H01L21/02562Tellurides
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/08Electroplating with moving electrolyte e.g. jet electroplating
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10Electroplating with more than one layer of the same or of different metals
    • C25D5/12Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00Electroplating characterised by the article coated
    • C25D7/12Semiconductors
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02367Substrates
    • H01L21/02428Structure
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02612Formation types
    • H01L21/02617Deposition types
    • H01L21/02623Liquid deposition
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemically Coating (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Weting (AREA)

Abstract

The invention discloses a tellurium-cadmium-mercury liquid-phase epitaxial growth source substrate which comprises a substrate body and a complex plating layer, wherein the complex plating layer is arranged on the substrate body, and a window for liquid-phase epitaxial growth of tellurium-cadmium-mercury is arranged between the complex plating layer and the substrate body. Also discloses a preparation method of the tellurium-cadmium-mercury liquid phase epitaxial growth source substrate and a tellurium-cadmium-mercury liquid phase epitaxial growth method based on the substrate. The substrate can effectively solve the problems that before mother solution is contacted with the substrate and in the epitaxial growth process of the tellurium-cadmium-mercury film, the temperature of each point on an interface is reduced due to uneven temperature field, the heat conductivity coefficient of a transmission substrate material can not well meet the temperature control conduction requirement and the like; and tellurium-cadmium-mercury liquid phase epitaxy on the substrate has quite good thickness uniformity, surface flatness, high single crystal property and lower half-peak width.

Description

Tellurium-cadmium-mercury liquid phase epitaxial growth source substrate and preparation method thereof, and tellurium-cadmium-mercury liquid phase epitaxial growth method
Technical Field
The invention belongs to the technical field of tellurium-cadmium-mercury liquid phase epitaxial growth, and particularly relates to a tellurium-cadmium-mercury liquid phase epitaxial growth source substrate, a preparation method thereof and a tellurium-cadmium-mercury liquid phase epitaxial growth method based on the substrate.
Background
Mercury cadmium telluride is an important II-VI compound semiconductor, has excellent photoelectric performance, and the room temperature nuclear radiation detector prepared from the mercury cadmium telluride is widely applied to the fields of X-ray spectrum analysis, medical imaging, industrial control, security guard detection, basic scientific research and the like, and has wide application prospect and immeasurable market value.
The temperature in the liquid phase epitaxy growth source of the tellurium-cadmium-mercury material has a great influence on the epitaxy growth rate, wherein the basic heat conductivity coefficient of the substrate is a necessary requirement on growth controllability of the tellurium-cadmium-mercury material, when the substrate is just contacted, the temperature of an epitaxy system is near a crystallization temperature, the temperature field is uneven, so that the actual temperature of an interface can be higher or lower than the crystallization temperature, the phenomenon of dissolution and supercooling growth can be caused, the crystallization temperature of mother liquor near the interface can be increased by dissolution, the initial growth speed can be accelerated by supercooling, and the initial conditions of epitaxial growth are complicated, so that the temperature of each point on the interface and the heat conductivity coefficient of the transmission substrate material can not well meet the requirement of temperature control conduction due to the uneven temperature field before the tellurium-cadmium-mercury mother liquor contacts with the substrate and in the process of epitaxial growth of the tellurium-cadmium-mercury film.
Disclosure of Invention
Aiming at the problems in the prior art, the substrate material of the tellurium-cadmium-mercury liquid-phase epitaxial growth source is provided for solving the problems that before the mother solution contacts with the substrate and in the process of epitaxial growth of the tellurium-cadmium-mercury thin film, the temperature field is uneven so that each point on the interface is cooled, and the heat conductivity coefficient of the transmission substrate material can not well meet the requirement of temperature control conduction.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the tellurium-cadmium-mercury liquid-phase epitaxial growth source substrate comprises a substrate body and a complex plating layer, wherein the complex plating layer is arranged on the substrate body, and a window for liquid-phase epitaxial growth of tellurium-cadmium-mercury is arranged between the complex plating layer and the substrate body. Namely, a window for liquid phase epitaxial growth of tellurium, cadmium and mercury is formed in the complex plating layer, and the window extends to the surface of the substrate body.
Preferably, the complex plating layer is a multilayer complex plating layer; preferably, the multilayer complex plating layer is a copper/nickel complex plating layer; preferably, the thickness of the multilayer complex plating layer is 50-100 mu m; preferably, the molar ratio of copper to nickel in the copper/nickel complex plating layer is 2-10:5-8.
Preferably, the copper/nickel complex plating layer is a complex plating layer of copper and nickel alternately; the copper/nickel complex plating layer is formed by alternately depositing copper layers and nickel layers on a tellurium-zinc-cadmium substrate by a spray electrodeposition method.
Preferably, the substrate body is a tellurium zinc cadmium substrate; the resistivity of the tellurium-zinc-cadmium substrate is 108-148 omega-m.
As a general inventive concept, there is also provided a method for preparing a mercury cadmium telluride liquid phase epitaxial growth source substrate, comprising the steps of:
(1) Preparing a substrate body;
(2) Coating a fluoride coating layer on a lattice growth surface area of the substrate body for epitaxially growing tellurium, cadmium and mercury;
(3) Depositing a complex plating layer on the surfaces of the substrate body and the fluoride coating layer;
(4) And removing the complex plating layer and the fluoride coating layer corresponding to the lattice growth surface area, and forming a window for epitaxially growing tellurium-cadmium-mercury on the substrate body.
Preferably, in the step (3), the complex plating layer is a multilayer complex plating layer, and the multilayer complex plating layer is a copper/nickel complex plating layer; the multilayer complex plating layer is alternately deposited on the tellurium-zinc-cadmium substrate body and the fluoride coating layer by a spray electrodeposition method; the deposition method of the multilayer complex plating layer specifically comprises the following steps: respectively adding the prepared copper solution and nickel solution into corresponding plating solution spray heads, then shooting the plating solution spray heads to the surfaces of the tellurium-zinc-cadmium substrate body and the fluoride coating layer, and repeatedly performing alternate spray deposition to form a copper and nickel complex plating layer; the method comprises the steps of carrying out a first treatment on the surface of the The thickness of the spray deposition is 50-100 mu m.
Preferably, in the step (2), the fluoride coating layer is coated by using a mask process, which specifically includes: and covering the lattice growth surface area except for the lattice growth surface area for epitaxially growing tellurium, cadmium and mercury on the substrate body by using a mask plate, and then coating a fluoride coating layer on the lattice growth surface area.
In the step (1), the substrate body is a tellurium-zinc-cadmium substrate; the preparation of the substrate comprises: the crystal phase surface of the tellurium zinc cadmium substrate 111 was ground and polished with 1% bromomethanol, then rinsed with isopropyl alcohol solution and blow-dried by a nitrogen gun.
Preferably, in the step (4), the copper-nickel complex plating layer on the lattice surface of the area to be grown on the surface of the substrate is etched by using etching liquid, wherein the etching liquid is aqueous solution of hydrochloric acid, nitric acid and a cupric ion source, the mass percent of hydrochloric acid is 10-15%, the mass percent of nitric acid is 1-10%, the mass percent of cupric ion is 0.001-0.01%, the cupric ion source can be provided by copper sulfate or copper oxide, fluoride can be removed by a distillation method under 130-135 ℃ through distilled water, and after removal, the copper-nickel complex plating layer can be cleaned by adopting an organic solvent, and the organic solvent is acetone, absolute ethyl alcohol and methanol.
Preferably, the area coated with the fluorinated coating is located at the center of the surface lattice growth 111 plane of the substrate body.
As a general inventive concept, the invention also provides a tellurium-cadmium-mercury liquid phase epitaxial growth method, which comprises the following steps:
s1, loading the tellurium-cadmium-mercury liquid phase epitaxial growth source substrate or the tellurium-cadmium-mercury liquid phase epitaxial growth source substrate prepared by the preparation method into an epitaxial graphite boat;
s2, synthesizing an epitaxial mother solution by adopting tellurium, cadmium and mercury raw materials, adopting mercury telluride as mercury compensation, and loading a proper amount of epitaxial mother solution and mercury telluride into an epitaxial graphite boat;
s3, controlling an initial temperature field and a growth process temperature field of the graphite boat to enable the epitaxial mother solution to carry out liquid phase epitaxy on the lattice surface of the substrate surface.
Preferably, the step S1 further comprises the step of cleaning the tellurium-cadmium-mercury liquid phase epitaxial growth source substrate by an organic solvent, wherein the organic solvent is acetone, absolute ethyl alcohol and methanol.
Compared with the prior art, the invention has the following advantages:
according to the invention, the copper and nickel multilayer complex plating film is prepared on the tellurium-zinc-cadmium lining substrate by utilizing the spray electrodeposition method, so that the temperature field control capability of tellurium-cadmium-mercury mother liquor when the tellurium-cadmium-mercury mother liquor is contacted with the substrate can be effectively improved during the operation of a tellurium-cadmium-mercury liquid phase epitaxial growth source, and the uniform heat conduction treatment capability of each point on the surface of the substrate is ensured, thereby meeting the requirement on temperature control conduction and being beneficial to improving the surface integrity of the tellurium-cadmium-mercury film through temperature control; the prepared complex plating layer can enable the tellurium-zinc-cadmium lining substrate to have higher hardness, stronger corrosion resistance and better wear resistance, so that the physical strength of the tellurium-cadmium-mercury lining is enhanced through the copper-nickel multilayer complex film, and the corresponding mechanical property is improved. The tellurium-cadmium-mercury epitaxial film grown by liquid phase epitaxy of the substrate has quite good thickness uniformity, surface flatness, high single crystal property and lower half-peak width.
Drawings
FIG. 1 is a flow chart of a liquid phase epitaxy growth source substrate process of the invention.
Fig. 2 is a diagram showing a structure of a substrate preparation of a liquid phase epitaxial growth source according to the present invention.
FIG. 3 is a schematic diagram of the processing of a multi-layer complex layer of a deposited tellurium-zinc-cadmium substrate in accordance with the present invention.
Fig. 4 is a coated stop fluorinated coating reticle.
In fig. 5, (a) is a test chart of the surface flatness of the mercury cadmium telluride epitaxial film obtained in example 3, and (b) is a test chart of the surface flatness of the mercury cadmium telluride epitaxial film obtained in comparative example 1.
Reference numerals:
1. copper-nickel complex plating; 2. a fluorinated coating layer; 3. a tellurium-zinc-cadmium substrate; 4. copper and nickel plating solution spray heads.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The substrate of the tellurium-cadmium-mercury liquid-phase epitaxial growth source comprises a tellurium-zinc-cadmium substrate and a multilayer complex plating layer, wherein the multilayer complex plating layer is loaded on the top of the tellurium-zinc-cadmium substrate body, the multilayer complex plating layer is alternately deposited on the top of the tellurium-zinc-cadmium substrate body through a jet electrodeposition method, the multilayer complex plating layer is a copper/nickel complex plating layer, the molar ratio of copper to nickel is 2:8, the substrate body is the tellurium-zinc-cadmium substrate, the tellurium-zinc-cadmium size is 2cm multiplied by 3cm, and the resistivity of the tellurium-zinc-cadmium substrate is 108-148 omega.m.
The specific process flow diagram of the substrate of the tellurium-cadmium-mercury liquid phase epitaxial growth source is shown in fig. 1, and the preparation method comprises the following steps:
(1) The preparation method of the tellurium-zinc-cadmium substrate comprises the following steps: the crystal phase surface of the tellurium zinc cadmium substrate 111 is ground, polished, ground and polished by 1% bromomethanol, then is flushed by isopropanol solution and dried by a nitrogen gun, a certain oxygen pressure is set outside electroplating equipment, and a copper and nickel multilayer complex film is sprayed and deposited by taking the tellurium zinc cadmium substrate as a base, wherein the resistivity of the tellurium zinc cadmium substrate is 108-148 omega m;
(2) Coating a fluorinated coating layer on the lattice growth surface of the substrate body by adopting masking; the area of the fluoride coating is 1.6cm multiplied by 2.4cm, the fluoride coating is blocked by a mask plate, the length, width and height of the mask plate are 3.2cm, 2.2cm and 2cm respectively, and the coating area is 1.6cm multiplied by 2.4cm, as shown in figure 4; the fluoride may be calcium fluoride or sodium fluoride.
(3) The method for processing and depositing the tellurium-zinc-cadmium substrate multilayer complex coating is shown in fig. 3, and specifically comprises the following steps: respectively adding the prepared copper solution and nickel solution into corresponding plating solution spray heads, spraying the composite plating solution to the surface of the substrate body and the surface of the fluorinated coating layer through the spray heads of a spray gun, enabling the spray gun to linearly reciprocate through a plating solution platform driving piece control seat, and repeatedly performing alternate spraying and deposition on the liquid spray heads at two sides to form the copper-nickel composite plating solution; the thickness of the spray-deposited copper and nickel complex plating layer is 50-100 mu m, so that the copper and nickel complex plating layer is sprayed on the surfaces of the substrate body and the fluorinated coating layer, and the obtained substrate preparation structure diagram is shown in figure 2; etching and corroding a copper-nickel complex plating layer on a lattice surface of a region to be grown on the surface of a substrate by using etching liquid, wherein the etching liquid is aqueous solution of hydrochloric acid, nitric acid and a cupric ion source, the mass percent of hydrochloric acid is 10-15%, the mass percent of nitric acid is 1-10%, the mass percent of cupric ion is 0.001-0.01%, the cupric ion source is provided by adopting copper sulfate, the surface layer of the copper-nickel complex plating layer in a growing range is removed by using the etching liquid, fluoride is removed by adopting a distillation method, the etching liquid is washed by distilled water, alcohol and acetone are then washed, and the corresponding growing lattice surface is exposed by washing.
The tellurium-cadmium-mercury liquid phase epitaxial growth method based on the tellurium-cadmium-mercury liquid phase epitaxial growth source substrate specifically comprises the following steps:
s1, improving the corresponding thickness of an epitaxial graphite boat according to the thickness of a multi-layer complex plating tellurium-zinc-cadmium substrate;
s2, cleaning the tellurium-zinc-cadmium substrate layer, and then loading the cleaned tellurium-zinc-cadmium substrate layer into an epitaxial graphite boat;
s3, synthesizing an epitaxial mother solution by adopting tellurium, cadmium and mercury raw materials, weighing a proper amount of epitaxial mother solution and mercury telluride, and loading the epitaxial mother solution and the mercury telluride into an epitaxial graphite boat for liquid phase epitaxy;
s4, controlling an initial temperature field and a growth process temperature field of the graphite boat, and forming a tellurium-cadmium-mercury epitaxial film by using the epitaxial mother solution.
Example 2
In one embodiment, the invention also provides a tellurium-zinc-cadmium liquid phase epitaxial growth source substrate, which comprises a tellurium-zinc-cadmium substrate and a multilayer complex plating layer, wherein the multilayer complex plating layer is loaded on the top of the tellurium-zinc-cadmium substrate, the multilayer complex plating layer is alternately deposited on the top of the tellurium-zinc-cadmium substrate through a spray electrodeposition method, the multilayer complex plating layer is a copper/nickel complex plating layer, and the molar ratio of copper to nickel is 4:6.
The preparation method of the substrate of the tellurium-cadmium-mercury liquid phase epitaxial growth source comprises the following steps:
(1) The preparation method of the tellurium-zinc-cadmium substrate comprises the following steps: the crystal phase surface of the tellurium-zinc-cadmium substrate 111 is ground and polished by 1% bromomethanol, then is flushed by isopropanol solution and dried by a nitrogen gun, a certain oxygen pressure is set outside electroplating equipment, the tellurium-zinc-cadmium substrate is used as a base to spray and deposit a copper and nickel multilayer complex film, and the resistivity of the tellurium-zinc-cadmium substrate is 108-148 omega m.
(2) Coating a fluorinated coating layer on the lattice growth surface of the substrate body by adopting masking; the area of the fluoride coating is 1.6cm multiplied by 2.4cm, the fluoride coating is blocked by a mask plate, the length, width and height of the mask plate are 3.2cm, 2.2cm and 2cm respectively, and the coating area is 1.6cm multiplied by 2.4cm, as shown in figure 4; the fluoride may be calcium fluoride or sodium fluoride.
(3) The method for processing and depositing the tellurium-zinc-cadmium substrate multilayer complex coating is shown in fig. 3, and specifically comprises the following steps: respectively adding the prepared copper solution and nickel solution into corresponding plating solution spray heads, spraying the composite plating solution to the surface of the substrate body and the surface of the fluorinated coating layer through the spray heads of a spray gun, enabling the spray gun to linearly reciprocate through a plating solution platform driving piece control seat, and repeatedly performing alternate spraying and deposition on the liquid spray heads at two sides to form the copper-nickel composite plating solution; the thickness of the spray-deposited copper and nickel complex plating layer is 50-100 mu m, so that the copper and nickel complex plating layer is sprayed on the surfaces of the substrate body and the fluorinated coating layer, and the obtained substrate preparation structure diagram is shown in figure 2; etching and corroding a copper-nickel complex plating layer on a lattice surface of a region to be grown on the surface of a substrate by using etching liquid, wherein the etching liquid is aqueous solution of hydrochloric acid, nitric acid and a cupric ion source, the mass percent of hydrochloric acid is 10-15%, the mass percent of nitric acid is 1-10%, the mass percent of cupric ion is 0.001-0.01%, the cupric ion source is provided by adopting copper sulfate, the surface layer of the copper-nickel complex plating layer in a growing range is removed by using the etching liquid, fluoride is removed by adopting a distillation method, the etching liquid is washed by distilled water, alcohol and acetone are then washed, and the corresponding growing lattice surface is exposed by washing.
The tellurium-cadmium-mercury liquid phase epitaxial growth method specifically comprises the following steps:
s1, improving the corresponding thickness of an epitaxial graphite boat according to the thickness of a multi-layer complex plating tellurium-zinc-cadmium substrate;
s2, cleaning the multi-layer complex plating tellurium-zinc-cadmium substrate, and loading the cleaned substrate into an epitaxial graphite boat;
s3, synthesizing an epitaxial mother solution by adopting tellurium, cadmium and mercury raw materials, weighing a proper amount of epitaxial mother solution and mercury telluride, and loading the epitaxial mother solution and the mercury telluride into an epitaxial graphite boat for liquid phase epitaxy;
s4, controlling an initial temperature field and a growth process temperature field of the graphite boat, and forming a tellurium-cadmium-mercury epitaxial film by using the epitaxial mother solution.
Example 3
In one embodiment, the invention also provides a substrate material of the tellurium-zinc-cadmium liquid phase epitaxial growth source, which comprises a tellurium-zinc-cadmium substrate and a multi-layer complex plating layer, wherein the multi-layer complex plating layer is loaded on the top of the tellurium-zinc-cadmium substrate, the multi-layer complex plating layer is alternately deposited on the top of the tellurium-zinc-cadmium substrate through a spray electrodeposition method, the multi-layer complex plating layer is a copper/nickel complex plating layer, and the molar ratio of copper to nickel is 7:5.
The preparation method of the substrate of the tellurium-cadmium-mercury liquid phase epitaxial growth source comprises the following steps:
(1) The preparation method of the tellurium-zinc-cadmium substrate comprises the following steps: the crystal phase surface of the tellurium-zinc-cadmium substrate 111 is ground and polished by 1% bromomethanol, then is flushed by isopropanol solution and dried by a nitrogen gun, a certain oxygen pressure is set outside electroplating equipment, the tellurium-zinc-cadmium substrate is used as a base to spray and deposit a copper and nickel multilayer complex film, and the resistivity of the tellurium-zinc-cadmium substrate is 108-148 omega m.
(2) Coating a fluorinated coating layer on the lattice growth surface of the substrate body by adopting masking; the area of the fluoride coating is 1.6cm multiplied by 2.4cm, the fluoride coating is blocked by a mask plate, the length, width and height of the mask plate are 3.2cm, 2.2cm and 2cm respectively, and the coating area is 1.6cm multiplied by 2.4cm, as shown in figure 4; the fluoride may be calcium fluoride or sodium fluoride.
(3) The method for processing and depositing the tellurium-zinc-cadmium substrate multilayer complex coating is shown in fig. 3, and specifically comprises the following steps: respectively adding the prepared copper solution and nickel solution into corresponding plating solution spray heads, spraying the composite plating solution to the surface of the substrate body and the surface of the fluorinated coating layer through the spray heads of a spray gun, enabling the spray gun to linearly reciprocate through a plating solution platform driving piece control seat, and repeatedly performing alternate spraying and deposition on the liquid spray heads at two sides to form the copper-nickel composite plating solution; the thickness of the spray-deposited copper and nickel complex plating layer is 50-100 mu m, so that the copper and nickel complex plating layer is sprayed on the surfaces of the substrate body and the fluorinated coating layer, and the obtained substrate preparation structure diagram is shown in figure 2; etching and corroding a copper-nickel complex plating layer on a lattice surface of a region to be grown on the surface of a substrate by using etching liquid, wherein the etching liquid is aqueous solution of hydrochloric acid, nitric acid and a cupric ion source, the mass percent of hydrochloric acid is 10-15%, the mass percent of nitric acid is 1-10%, the mass percent of cupric ion is 0.001-0.01%, the cupric ion source is provided by adopting copper sulfate, the surface layer of the copper-nickel complex plating layer in a growing range is removed by using the etching liquid, fluoride is removed by adopting a distillation method, the etching liquid is washed by distilled water, alcohol and acetone are then washed, and the corresponding growing lattice surface is exposed by washing.
The tellurium-cadmium-mercury liquid phase epitaxial growth method specifically comprises the following steps:
s1, improving the corresponding thickness of an epitaxial graphite boat according to the thickness of a multi-layer complex plating tellurium-zinc-cadmium substrate;
s2, cleaning the tellurium-zinc-cadmium substrate with the multilayer complex plating layer, and then loading the substrate into an epitaxial graphite boat;
s3, synthesizing an epitaxial mother solution by adopting tellurium, cadmium and mercury raw materials, weighing a proper amount of epitaxial mother solution and mercury telluride, and loading the epitaxial mother solution and the mercury telluride into an epitaxial graphite boat for liquid phase epitaxy;
s4, controlling an initial temperature field and a growth process temperature field of the graphite boat, and forming a tellurium-cadmium-mercury epitaxial film by using the epitaxial mother solution.
Example 4
In one embodiment, the invention also provides a substrate material of the tellurium-zinc-cadmium liquid phase epitaxial growth source, which comprises a tellurium-zinc-cadmium substrate and a multi-layer complex plating layer, wherein the multi-layer complex plating layer is loaded on the top of the tellurium-zinc-cadmium substrate, the multi-layer complex plating layer is alternately deposited on the top of the tellurium-zinc-cadmium substrate through a spray electrodeposition method, the multi-layer complex plating layer is a copper/nickel complex plating layer, and the molar ratio of copper to nickel is 10:5.
The preparation method of the substrate of the tellurium-cadmium-mercury liquid phase epitaxial growth source comprises the following steps:
(1) The preparation method of the tellurium-zinc-cadmium substrate comprises the following steps: the crystal phase surface of the tellurium-zinc-cadmium substrate 111 is ground and polished by 1% bromomethanol, then is flushed by isopropanol solution and dried by a nitrogen gun, a certain oxygen pressure is set outside electroplating equipment, the tellurium-zinc-cadmium substrate is used as a base to spray and deposit a copper and nickel multilayer complex film, and the resistivity of the tellurium-zinc-cadmium substrate is 108-148 omega m.
(2) Coating a fluorinated coating layer on the lattice growth surface of the substrate body by adopting masking; the area of the fluoride coating is 1.6cm multiplied by 2.4cm, the fluoride coating is blocked by a mask plate, the length, width and height of the mask plate are 3.2cm, 2.2cm and 2cm respectively, and the coating area is 1.6cm multiplied by 2.4cm, as shown in figure 4; the fluoride may be calcium fluoride or sodium fluoride.
(3) The method for processing and depositing the tellurium-zinc-cadmium substrate multilayer complex coating is shown in fig. 3, and specifically comprises the following steps: respectively adding the prepared copper solution and nickel solution into corresponding plating solution spray heads, spraying the composite plating solution to the surface of the substrate body and the surface of the fluorinated coating layer through the spray heads of a spray gun, enabling the spray gun to linearly reciprocate through a plating solution platform driving piece control seat, and repeatedly performing alternate spraying and deposition on the liquid spray heads at two sides to form the copper-nickel composite plating solution; the thickness of the spray-deposited copper and nickel complex plating layer is 50-100 mu m, so that the copper and nickel complex plating layer is sprayed on the surfaces of the substrate body and the fluorinated coating layer, and the obtained substrate preparation structure diagram is shown in figure 2; etching and corroding a copper-nickel complex plating layer on a lattice surface of a region to be grown on the surface of a substrate by using etching liquid, wherein the etching liquid is aqueous solution of hydrochloric acid, nitric acid and a cupric ion source, the mass percent of hydrochloric acid is 10-15%, the mass percent of nitric acid is 1-10%, the mass percent of cupric ion is 0.001-0.01%, the cupric ion source is provided by copper sulfate, the surface layer of the copper-nickel complex plating layer in a growing range is removed by using the etching liquid, fluoride is removed by using a distillation method, the fluoride is washed by using distilled water, then the solution is washed by alcohol and acetone, and the corresponding growing lattice surface is exposed by washing.
The tellurium-cadmium-mercury liquid phase epitaxial growth method specifically comprises the following steps:
s1, improving the corresponding thickness of an epitaxial graphite boat according to the thickness of a multi-layer complex plating tellurium-zinc-cadmium substrate;
s2, cleaning the tellurium-zinc-cadmium substrate with the multilayer complex plating layer, and then loading the substrate into an epitaxial graphite boat;
s3, synthesizing an epitaxial mother solution by adopting tellurium, cadmium and mercury raw materials, weighing a proper amount of epitaxial mother solution and mercury telluride, and loading the epitaxial mother solution and the mercury telluride into an epitaxial graphite boat for liquid phase epitaxy;
s4, controlling an initial temperature field and a growth process temperature field of the graphite boat, and forming a tellurium-cadmium-mercury epitaxial film by using the epitaxial mother solution.
Comparative example 1
A substrate of a tellurium-zinc-cadmium liquid phase epitaxial growth source is a tellurium-zinc-cadmium substrate.
The specific processing method of the tellurium-zinc-cadmium substrate comprises the following steps: the crystal phase surface of the tellurium-zinc-cadmium substrate 111 is ground and polished by 1% bromomethanol, then is washed by isopropanol solution and is dried by a nitrogen gun, and the resistivity of the tellurium-zinc-cadmium substrate is 108-148 omega m;
the lattice growth surface of the tellurium-zinc-cadmium substrate is 111, and the area of the lattice growth surface is 2cm multiplied by 3cm.
The tellurium-cadmium-mercury liquid phase epitaxial growth method specifically comprises the following steps:
s1, cleaning the tellurium-zinc-cadmium substrate, and then loading the substrate into an epitaxial graphite boat;
s2, synthesizing an epitaxial mother solution by adopting tellurium, cadmium and mercury raw materials, weighing a proper amount of epitaxial mother solution and mercury telluride for mercury compensation, and loading the epitaxial mother solution and the mercury telluride into an epitaxial graphite boat for liquid phase epitaxy;
s3, controlling an initial temperature field and a growth process temperature field of the graphite boat, and forming a tellurium-cadmium-mercury epitaxial film by using the epitaxial mother solution.
Characterization of the prepared tellurium-cadmium-mercury epitaxial film is carried out, as shown in fig. 5, wherein (a) is a test chart of the surface flatness of the tellurium-cadmium-mercury epitaxial film obtained by liquid phase epitaxy in example 3, and (b) is a test chart of the surface flatness of the tellurium-cadmium-mercury epitaxial film obtained by liquid phase epitaxy in comparative example 1, and as can be seen from fig. 5, the flatness of the tellurium-cadmium-mercury epitaxial film obtained by epitaxial growth is obviously improved compared with a substrate without an alloy plating layer.
The thicknesses of the workpieces before and after electrodeposition of the epitaxial growth source substrates prepared in examples 1 to 4 and comparative example 1 were measured by a laser thickness meter to calculate the thickness of the plating layer, the friction factors of the plating layers after polishing were measured and compared by a frictional wear testing machine, the calculated wear amounts were weighed, and the corresponding thermal conductivity was measured, and the measured performance parameters are shown in table 1:
TABLE 1
From the above table, example 3 is a preferred embodiment of the present invention, and the thermal conductivity, the thickness of the plating layer, the relative mean square error of the distribution of the material component surfaces and the relative mean square error of the thickness are all optimal treatments, and the transmittance reaches 56% as measured by an infrared fourier spectrometer under the condition that the molar ratio of copper to nickel is 7:5.
The above-mentioned embodiments are only preferred embodiments of the present invention, but the protection scope of the present invention is not limited thereto, and the area, area and shape of the coated fluoride can be changed according to the product utilization requirement in actual processing, and any person skilled in the art should be able to apply equivalent substitutions or alterations according to the technical solution and the inventive concept of the present invention within the protection scope of the present invention.

Claims (10)

1. The tellurium-cadmium-mercury liquid-phase epitaxial growth source substrate is characterized by comprising a substrate body and a complex plating layer, wherein the complex plating layer is arranged on the substrate body, and a window for liquid-phase epitaxial growth of tellurium-cadmium-mercury is arranged between the complex plating layer and the substrate body; the complex plating layer is a multilayer complex plating layer; the multilayer complex plating layer is a copper/nickel complex plating layer.
2. The tellurium-cadmium-mercury liquid phase epitaxial growth source substrate of claim 1, wherein the thickness of the multilayer complex plating layer is 50-100 μm; the molar ratio of copper to nickel in the copper/nickel complex plating layer is 2-10:5-8.
3. The tellurium-cadmium-mercury liquid phase epitaxial growth source substrate of claim 2, wherein the copper/nickel complex plating is copper-nickel alternating complex plating; the copper/nickel complex plating layer is formed by alternately depositing copper layers and nickel layers on a tellurium-zinc-cadmium substrate by a spray electrodeposition method.
4. A mercury cadmium telluride liquid phase epitaxial growth source substrate according to any one of claims 1 to 3 wherein the substrate body is a cadmium zinc telluride substrate; the resistivity of the tellurium-zinc-cadmium substrate is 108-148 omega-m.
5. The method for preparing a mercury cadmium telluride liquid phase epitaxial growth source substrate according to any one of claims 1 to 4, comprising the steps of:
(1) Preparing a substrate body;
(2) Coating a fluoride coating layer on a lattice growth surface area of the substrate body for epitaxially growing tellurium, cadmium and mercury;
(3) Depositing a complex plating layer on the surfaces of the substrate body and the fluoride coating layer;
(4) And removing the complex plating layer and the fluoride coating layer corresponding to the lattice growth surface area, and forming a window for epitaxially growing tellurium-cadmium-mercury on the substrate body.
6. The method for preparing a mercury cadmium telluride liquid phase epitaxial growth source substrate according to claim 5 wherein in step (3), the complex plating layer is a multilayer complex plating layer, and the multilayer complex plating layer is a copper/nickel complex plating layer; the multilayer complex plating layer is alternately deposited on the tellurium-zinc-cadmium substrate body and the fluoride coating layer by a spray electrodeposition method; the deposition method of the multilayer complex plating layer specifically comprises the following steps: respectively adding the prepared copper solution and nickel solution into corresponding plating solution spray heads, then shooting the plating solution spray heads to the surfaces of the tellurium-zinc-cadmium substrate body and the fluoride coating layer, and repeatedly performing alternate spray deposition to form a copper and nickel complex plating layer; the thickness of the spray deposition is 50-100 mu m.
7. The method for preparing a mercury cadmium telluride liquid phase epitaxial growth source substrate according to claim 5, wherein in step (2), the fluoride coating layer is coated by using a mask process, specifically comprising: and covering the lattice growth surface area except for the lattice growth surface area for epitaxially growing tellurium, cadmium and mercury on the substrate body by using a mask plate, and then coating a fluoride coating layer on the lattice growth surface area.
8. The method for preparing a mercury cadmium telluride liquid phase epitaxial growth source substrate according to claim 5 wherein the area coated with the fluorinated coating is located at the center of the 111 facets of the growth of the surface lattice of the substrate body.
9. The method for preparing a mercury cadmium telluride liquid phase epitaxial growth source substrate according to claim 5, wherein in step (4), etching the copper-nickel complex plating layer on the lattice surface of the area to be grown on the surface of the substrate by using an etching solution, wherein the etching solution is aqueous solution of hydrochloric acid, nitric acid and a cupric ion source; in the etching solution, the mass percentage of hydrochloric acid is 10-15%, the mass percentage of nitric acid is 1-10%, and the mass percentage of cupric ions is 0.001-0.01%; the fluoride is removed by distillation.
10. The tellurium-cadmium-mercury liquid phase epitaxial growth method is characterized by comprising the following steps of:
s1, loading a tellurium-cadmium-mercury liquid phase epitaxial growth source substrate prepared by any one of claims 1-4 or a tellurium-cadmium-mercury liquid phase epitaxial growth source substrate prepared by the preparation method of any one of claims 5-9 into an epitaxial graphite boat;
s2, synthesizing an epitaxial mother solution by adopting tellurium, cadmium and mercury raw materials, adopting mercury telluride as mercury compensation, and loading a proper amount of epitaxial mother solution and mercury telluride into an epitaxial graphite boat;
s3, controlling an initial temperature field and a growth process temperature field of the graphite boat to enable the epitaxial mother solution to carry out liquid phase epitaxy on the lattice surface of the substrate surface.
CN202111070423.7A 2021-09-13 2021-09-13 Tellurium-cadmium-mercury liquid phase epitaxial growth source substrate and preparation method thereof, and tellurium-cadmium-mercury liquid phase epitaxial growth method Active CN113782416B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111070423.7A CN113782416B (en) 2021-09-13 2021-09-13 Tellurium-cadmium-mercury liquid phase epitaxial growth source substrate and preparation method thereof, and tellurium-cadmium-mercury liquid phase epitaxial growth method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111070423.7A CN113782416B (en) 2021-09-13 2021-09-13 Tellurium-cadmium-mercury liquid phase epitaxial growth source substrate and preparation method thereof, and tellurium-cadmium-mercury liquid phase epitaxial growth method

Publications (2)

Publication Number Publication Date
CN113782416A CN113782416A (en) 2021-12-10
CN113782416B true CN113782416B (en) 2024-03-05

Family

ID=78843120

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111070423.7A Active CN113782416B (en) 2021-09-13 2021-09-13 Tellurium-cadmium-mercury liquid phase epitaxial growth source substrate and preparation method thereof, and tellurium-cadmium-mercury liquid phase epitaxial growth method

Country Status (1)

Country Link
CN (1) CN113782416B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114753008B (en) * 2022-03-29 2023-04-28 中国电子科技集团公司第十一研究所 Method for preparing tellurium-zinc-cadmium substrate with adjustable zinc components and uniform distribution
CN116482150B (en) * 2023-06-25 2023-09-12 浙江珏芯微电子有限公司 Tellurium-cadmium-mercury doping activation rate evaluation method

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1988001309A1 (en) * 1986-08-15 1988-02-25 Massachusetts Institute Of Technology Method for forming a metal coating on a substrate
US4735662A (en) * 1987-01-06 1988-04-05 The Standard Oil Company Stable ohmic contacts to thin films of p-type tellurium-containing II-VI semiconductors
US5399503A (en) * 1989-07-19 1995-03-21 Fujitsu Limited Method for growing a HgCdTe epitaxial layer on a semiconductor substrate
CN101109105A (en) * 2007-08-22 2008-01-23 中国科学院上海技术物理研究所 Graphite boat for improving mercury cadmium telluride rheotaxy membrane surface shape
CN101348941A (en) * 2008-09-02 2009-01-21 中国电子科技集团公司第十一研究所 Substrate material for mercury cadmium telluride material growth by liquid phase epitaxy method and preparation thereof
CN104867837A (en) * 2015-01-21 2015-08-26 中国科学院上海技术物理研究所 Composite mask for high energy ion implantation
CN110277468A (en) * 2019-06-26 2019-09-24 山东大学 A kind of preparation method of big size graphene/two dimension tellurides hetero-junctions infrared photoelectric detector

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1988001309A1 (en) * 1986-08-15 1988-02-25 Massachusetts Institute Of Technology Method for forming a metal coating on a substrate
US4735662A (en) * 1987-01-06 1988-04-05 The Standard Oil Company Stable ohmic contacts to thin films of p-type tellurium-containing II-VI semiconductors
US5399503A (en) * 1989-07-19 1995-03-21 Fujitsu Limited Method for growing a HgCdTe epitaxial layer on a semiconductor substrate
CN101109105A (en) * 2007-08-22 2008-01-23 中国科学院上海技术物理研究所 Graphite boat for improving mercury cadmium telluride rheotaxy membrane surface shape
CN101348941A (en) * 2008-09-02 2009-01-21 中国电子科技集团公司第十一研究所 Substrate material for mercury cadmium telluride material growth by liquid phase epitaxy method and preparation thereof
CN104867837A (en) * 2015-01-21 2015-08-26 中国科学院上海技术物理研究所 Composite mask for high energy ion implantation
CN110277468A (en) * 2019-06-26 2019-09-24 山东大学 A kind of preparation method of big size graphene/two dimension tellurides hetero-junctions infrared photoelectric detector

Also Published As

Publication number Publication date
CN113782416A (en) 2021-12-10

Similar Documents

Publication Publication Date Title
CN113782416B (en) Tellurium-cadmium-mercury liquid phase epitaxial growth source substrate and preparation method thereof, and tellurium-cadmium-mercury liquid phase epitaxial growth method
Selvamanickam et al. MOCVD-based YBCO-coated conductors
US20070232065A1 (en) Composition Control For Photovoltaic Thin Film Manufacturing
CN1274011C (en) Crystalline grain in metal film growth control method
US5873992A (en) Method of electroplating a substrate, and products made thereby
Zhang et al. A transmission electron microscopy and reflection high‐energy electron diffraction study of the initial stages of the heteroepitaxial growth of InSb on GaAs (001) by molecular beam epitaxy
CN106086812B (en) A kind of anti abrasive composite coating of metal surface anticorrosive and preparation method thereof
CN111276277A (en) Window with infrared transparent conductive function
Driver et al. The electronic and chemical structure of the a-B3CO0. 5: Hy-to-metal interface from photoemission spectroscopy: implications for Schottky barrier heights
CN107230735B (en) The preparation method of CdZnTe film photoelectric detector with buffer layer
Ozgit-Akgun et al. Plasma-enhanced atomic layer deposition of III-nitride thin films
Nakaoka et al. Improvement of production rate of YBCO coated conductors fabricated by TFA-MOD method
Tamulevičius et al. Stress and surface studies of SILAR grown CdS thin films on GaAs (100)
WO2010110870A1 (en) Photovoltaic cells with plated steel substrate
Parker et al. The stress of electroless nickel deposits on beryllium
Chihi et al. Correlation between microstructure and optical properties of cu (In0. 7, Ga0. 3) Se2 grown by electrodeposition technique
JP3544095B2 (en) Method for producing zinc oxide thin film, semiconductor device substrate and photovoltaic device using the same
EP3186823A1 (en) Exfoliation process for removal of deposited materials from masks carriers, and deposition tool components
CN116695091B (en) Hydrophobic conductive film and preparation method and application thereof
JP3115103B2 (en) Industrial material with fluorinated passivation film
Bocking et al. The structure of gold and gold alloys produced using high speed selective jet electrodeposition
Nakaoka et al. High-rate fabrication of YBCO coated conductors using TFA-MOD method
Salohub et al. Morphology, chemical composition and optical properties of Zn 2 SnO 4 films obtained by pulsed spray pyrolysis
RU2570715C2 (en) Method of forming light-absorbing coating
TWI768802B (en) Flexible copper clad laminate film, article including the same, and method of manufacturing the flexible copper clad laminate film

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant