CN106024625B - A kind of highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method - Google Patents
A kind of highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method Download PDFInfo
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- CN106024625B CN106024625B CN201610584312.0A CN201610584312A CN106024625B CN 106024625 B CN106024625 B CN 106024625B CN 201610584312 A CN201610584312 A CN 201610584312A CN 106024625 B CN106024625 B CN 106024625B
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- 239000002253 acid Substances 0.000 title claims abstract description 82
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 230000007797 corrosion Effects 0.000 claims abstract description 101
- 238000005260 corrosion Methods 0.000 claims abstract description 101
- 238000000465 moulding Methods 0.000 claims abstract description 54
- 238000002161 passivation Methods 0.000 claims abstract description 45
- 239000011521 glass Substances 0.000 claims abstract description 43
- 239000004020 conductor Substances 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 38
- 239000003518 caustics Substances 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 32
- 229910000679 solder Inorganic materials 0.000 claims abstract description 22
- 239000004411 aluminium Substances 0.000 claims abstract description 19
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 19
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 17
- 239000011733 molybdenum Substances 0.000 claims abstract description 17
- 238000009792 diffusion process Methods 0.000 claims abstract description 15
- 238000005538 encapsulation Methods 0.000 claims abstract description 13
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 13
- 239000010937 tungsten Substances 0.000 claims abstract description 13
- 238000005516 engineering process Methods 0.000 claims abstract description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 60
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 60
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 60
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 36
- 238000005245 sintering Methods 0.000 claims description 31
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 30
- 229960000583 acetic acid Drugs 0.000 claims description 30
- 239000012362 glacial acetic acid Substances 0.000 claims description 30
- 229910017604 nitric acid Inorganic materials 0.000 claims description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 29
- 229910002804 graphite Inorganic materials 0.000 claims description 29
- 239000010439 graphite Substances 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 28
- 238000003466 welding Methods 0.000 claims description 26
- 229910052751 metal Inorganic materials 0.000 claims description 25
- 239000002184 metal Substances 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 23
- 238000005530 etching Methods 0.000 claims description 21
- 230000008018 melting Effects 0.000 claims description 18
- 238000002844 melting Methods 0.000 claims description 18
- 238000004140 cleaning Methods 0.000 claims description 17
- 238000010410 dusting Methods 0.000 claims description 14
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 150000002500 ions Chemical class 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- 241000209140 Triticum Species 0.000 claims description 7
- 235000021307 Triticum Nutrition 0.000 claims description 7
- 238000005219 brazing Methods 0.000 claims description 7
- 238000005566 electron beam evaporation Methods 0.000 claims description 7
- 235000013312 flour Nutrition 0.000 claims description 7
- 229910052709 silver Inorganic materials 0.000 claims description 7
- 239000004332 silver Substances 0.000 claims description 7
- 239000012459 cleaning agent Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 230000005684 electric field Effects 0.000 claims description 5
- 230000008014 freezing Effects 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims description 3
- 238000003780 insertion Methods 0.000 claims description 3
- 230000037431 insertion Effects 0.000 claims description 3
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 230000005855 radiation Effects 0.000 abstract description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 22
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 230000002779 inactivation Effects 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 230000002378 acidificating effect Effects 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 239000010949 copper Substances 0.000 description 8
- 238000000227 grinding Methods 0.000 description 8
- 239000003643 water by type Substances 0.000 description 8
- 230000005611 electricity Effects 0.000 description 5
- 101100373011 Drosophila melanogaster wapl gene Proteins 0.000 description 4
- 239000007853 buffer solution Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 210000004483 pasc Anatomy 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 241000790917 Dioxys <bee> Species 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- MGRWKWACZDFZJT-UHFFFAOYSA-N molybdenum tungsten Chemical compound [Mo].[W] MGRWKWACZDFZJT-UHFFFAOYSA-N 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/66007—Multistep manufacturing processes
- H01L29/66075—Multistep manufacturing processes of devices having semiconductor bodies comprising group 14 or group 13/15 materials
- H01L29/66083—Multistep manufacturing processes of devices having semiconductor bodies comprising group 14 or group 13/15 materials the devices being controllable only by variation of the electric current supplied or the electric potential applied, to one or more of the electrodes carrying the current to be rectified, amplified, oscillated or switched, e.g. two-terminal devices
- H01L29/6609—Diodes
Landscapes
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Ceramic Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Ceramic Products (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Powder Metallurgy (AREA)
Abstract
A kind of highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method provided by the invention; using molybdenum or tungsten as contact conductor; tube core is using aluminium as solder; chip uses depth-diffusion process; table top moulding is orthogonal rake moulding, which reduces surface field, while before carrying out glassivation encapsulation; chip table is protected using acid, caustic corrosion technique and passivation technology, high temperature is then carried out using specific glass powder and is passivated encapsulated moulding;Chip of the present invention reduces the surface field of device at orthogonal rake, improves the stability of chip surface;Chip surface is cleaned to greatest extent in chip corrosion process, reduces the influence of interface charge, is made device that there is good avalanche breakdown performance, is promoted the reliability of product;Since passivation layer is thicker, while there is certain lead tolerance to enable product steady operation under radiation parameter.
Description
Technical field
The present invention relates to diode fabrication process more particularly to a kind of highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode
Manufacturing method.
Background technique
Semiconductor voltage adjustment diode (zener diode) be it is a kind of work breakdown conditions device, the present invention relates to
A kind of manufacturing method of highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode, greatly improve device uses field, produces
Product can be used in the extremely harsh Aeronautics and Astronautics field of environmental requirement.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diodes
Manufacturing method.
The present invention is achieved by the following technical programs.
A kind of highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method provided by the invention, using molybdenum or tungsten
As contact conductor, for tube core using aluminium as solder, chip uses depth-diffusion process, and table top moulding is orthogonal rake moulding, should
Chip structure reduces surface field, while before carrying out glassivation encapsulation, using acid, caustic corrosion technique and passivation technology to core
Piece table top is protected, and is then carried out high temperature using specific glass powder and is passivated encapsulated moulding;The specific steps are that:
A) PN junction is formed on monocrystalline silicon piece by deep method of diffusion of tying, then passes through the method for electron beam evaporation in PN junction
The face P and N wheat flour are for aluminium or the metal film layer of silver;
B) it is cut by blast and the monocrystalline silicon piece blast for being coated with metal film layer is molded into the pipe that section is trapezoidal table top
Core;
C) corrosion 14~16min of cleaning is carried out to the tube core of well cutting using cleaning agent, tube core after etching is with third
Ketone carries out 8~12min of ultrasonic cleaning, then carries out 8~12min of ultrasonic cleaning with alcohol, is then dehydrated, dries;
D) electrode and metal lead wire are freezed into the contact conductor of an entirety, then contact conductor, pipe by high temperature sintering
Core, contact conductor are successively vertically stacked in graphite jig, then graphite jig is put into contact conductor in vacuum sintering furnace and
Tube core carry out melting welding key and.
E) it is corroded using acid corrosion liquid in the diode insertion corrosion disk after freezing, is used after etching
Ionized water cleaning;
F) diode after acid corrosion is put into 3~5min of corrosion cleaning in caustic corrosion liquid, with hot and cold deionization after removal
Water alternately rinses 10 times;
G) diode after molding, which is put into the passivating solution that temperature is 55~60 DEG C, is passivated 1~3min;
H) diode after acid corrosion is loaded in graphite bar, automatic dusting and uniform coated particle degree is used on table top
Glass powder paste more than 800 mesh forms uniform sphere, is sent into low temperature moulding furnace after dusting and carries out 2~3h of molding.
The cleaning agent is 65%~68% nitric acid, >=40% hydrofluoric acid, 95%~98% by mass percentage
The mixed solution of sulfuric acid, >=99.5% glacial acetic acid 8:2:2:5 by volume.
The solder of the high temperature sintering is brazing piece, and high temperature sintering temperature is 800~900 DEG C.
Metallic film on the tube core is the solder of tube core key sum, and the temperature of melting welding key sum is 620~750 DEG C.
The acid corrosion liquid be by mass percentage analytically pure 65%~68% nitric acid, >=40% hydrofluoric acid,
The mixed solution of 95%~98% sulfuric acid, >=99.5% glacial acetic acid 12:9:12:6 by volume.
The potassium hydroxide solution that the caustic corrosion liquid is 3%~6%, caustic corrosion liquid temperature are 90~95 DEG C.
The passivating solution be by mass percentage >=30% hydrogen peroxide, >=85% hydrogen peroxide and ionized water by 2:2:5
Mixed mixed liquor.
In the glass powder containing 2%~10% lead, the coefficient of expansion is close with molybdenum, tungsten electrode.
The low temperature moulding furnace heating rate 10~15 DEG C/min, 45~65min of heating-up time, maximum sintering temperature 660
DEG C, 5~15min of constant temperature time, rate of temperature fall≤5 DEG C/min.
The beneficial effects of the present invention are: chip separation forms orthogonal rake using positive blast cutting mode, greatly reduces
The surface field of device improves the stability of chip surface;Chip table is removed using acid corrosion in chip corrosion process
Damaging layer, etching process removal be adhered to the heavy metal ion of chip surface, in thermal inactivation mode and alkali metal ion and in core
Piece surface grows the technique of layer of silicon dioxide passivation protection layer, cleans chip surface to greatest extent, reduces interface electricity
The influence of lotus makes device have good avalanche breakdown performance, promotes the reliability of product;Product use have it is certain it is leaded at
The glass powder divided realizes the passivation and encapsulation effect of product through high-temperature molding, since passivation layer is thicker, while having certain contain
Lead amount enables product steady operation under radiation parameter.The heat of molybdenum (tungsten) electrode and chip and glass passivation layer in product component
The coefficient of expansion is suitable, improves the thermal matching energy of product, while low temperature moulding is used in the forming process of product glass powder
Technique, heating, cooling rate is slower, can preferably discharge the stress in glass passivation layer, and device can be in -65~200 DEG C of temperature
It works under the conditions of degree, reliability with higher.
Specific embodiment
Be described further below technical solution of the present invention, but claimed range be not limited to it is described.
A kind of highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method, is drawn using molybdenum or tungsten as electrode
Line, for tube core using aluminium as solder, chip uses depth-diffusion process, and table top moulding is orthogonal rake moulding, chip structure drop
Low surface field, while before carrying out glassivation encapsulation, chip table is carried out using acid, caustic corrosion technique and passivation technology
Then protection carries out high temperature using specific glass powder and is passivated encapsulated moulding;The specific steps are that:
A) PN junction is formed on monocrystalline silicon piece by deep method of diffusion of tying, then passes through the method for electron beam evaporation in PN junction
The face P and N wheat flour are for aluminium or the metal film layer of silver;
B) it is cut by blast and the monocrystalline silicon piece blast for being coated with metal film layer is molded into the pipe that section is trapezoidal table top
Core;
C) corrosion 14~16min of cleaning is carried out to the tube core of well cutting using cleaning agent, tube core after etching is with third
Ketone carries out 8~12min of ultrasonic cleaning, then carries out 8~12min of ultrasonic cleaning with alcohol, is then dehydrated, dries;
D) electrode and metal lead wire are freezed into the contact conductor of an entirety, then contact conductor, pipe by high temperature sintering
Core, contact conductor are successively vertically stacked in graphite jig, then graphite jig is put into contact conductor in vacuum sintering furnace and
Tube core carry out melting welding key and.
E) it is corroded using acid corrosion liquid in the diode insertion corrosion disk after freezing, is used after etching
Ionized water cleaning;
F) diode after acid corrosion is put into 3~5min of corrosion cleaning in caustic corrosion liquid, with hot and cold deionization after removal
Water alternately rinses 10 times;
G) diode after acid corrosion, which is put into the passivating solution that temperature is 55~60 DEG C, is passivated 1~3min;
H) diode after passivation is loaded in graphite bar, is existed on table top using automatic dusting and uniform coated particle degree
Glass powder pastes more than 800 mesh forms uniform sphere, is sent into low temperature moulding furnace after dusting and carries out 2~3h of molding.
The cleaning agent is 65%~68% nitric acid, >=40% hydrofluoric acid, 95%~98% by mass percentage
The mixed solution of sulfuric acid, >=99.5% glacial acetic acid 8:2:2:5 by volume.
The solder of the high temperature sintering is brazing piece, and high temperature sintering temperature is 800~900 DEG C.
Metallic film on the tube core is the solder of tube core key sum, and the temperature of melting welding key sum is 620~750 DEG C.
The acid corrosion liquid be by mass percentage analytically pure 65%~68% nitric acid, >=40% hydrofluoric acid,
The mixed solution of 95%~98% sulfuric acid, >=99.5% glacial acetic acid 12:9:12:6 by volume.
The potassium hydroxide solution that the caustic corrosion liquid is 3%~6%, caustic corrosion liquid temperature are 90~95 DEG C.
The passivating solution be by mass percentage >=30% hydrogen peroxide, >=85% hydrogen peroxide and ionized water by 2:2:5
Mixed mixed liquor.
In the glass powder containing 2%~10% lead, the coefficient of expansion is close with molybdenum, tungsten electrode.
The low temperature moulding furnace heating rate 10~15 DEG C/min, 45~65min of heating-up time, maximum sintering temperature 660
DEG C, 5~15min of constant temperature time, rate of temperature fall≤5 DEG C/min.
Embodiment 1
A kind of highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method, using molybdenum as contact conductor, pipe
For core using aluminium as solder, chip uses depth-diffusion process, and table top moulding is orthogonal rake moulding, which reduces surface
Electric field, while before carrying out glassivation encapsulation, chip table is protected using acid, caustic corrosion technique and passivation technology,
Then high temperature is carried out using specific glass powder and is passivated encapsulated moulding;Step are as follows:
(1) tube core is prepared.PN junction, then the side for passing through electron beam evaporation are formed on monocrystalline silicon piece by deep method of diffusion of tying
Method, for aluminium or the metal film layer of silver, then is cut by blast in the face P of PN junction and N wheat flour and will be coated with the monocrystalline of metal film layer
The molding of silicon wafer blast becomes the tube core in bucking ladder face.
(2) corrosion cleaning tube core.The tube core of well cutting is carried out using the mixed acid of nitric acid, hydrofluoric acid, sulfuric acid, glacial acetic acid
Corrosion, nitric acid, hydrofluoric acid, sulfuric acid and glacial acetic acid mass percentage concentration be respectively as follows: in 65,40%, 95%, 99.5% mixed acid
Nitric acid, hydrofluoric acid, sulfuric acid and glacial acetic acid volume proportion be 8:2:2:5, etching time 14min, the tube core after etching
Primary, the time 10min that carries out ultrasonic cleaning with acetone, in primary, the time 10min that carries out ultrasonic cleaning with alcohol, then
Dehydration, drying.Cleaned by the corrosion of above-mentioned mixed acid, can effectively remove chip table mechanical damage layer and impurity from
Son.
(3) it freezes assembling.Using brazing piece as solder, by high temperature sintering methods by molybdenum or tungsten electrode and copper metal lead
Or welding wire welding lead forms whole contact conductor together, the temperature of high temperature sintering is 800 DEG C;Again by two electrodes
Lead and tube core are with being assembled into graphite jig, graphite grinding tool upper cover plate and lower cover plate, two contact conductors when combo
Electrode end surface is in close contact with the metallic film on the face P and the face N of tube core respectively, and contact conductor, tube core, contact conductor successively erect
It directly stacks, then graphite jig is put into vacuum sintering furnace, and contact conductor and tube core are subjected to melting welding bonding, aluminium at high temperature
The corresponding melting welding bonding temperature of metallic film is 640 DEG C, improves the quality of melting welding bonding.Metallic film on tube core is to realize electricity
The solder that pole lead is bonded with tube core, the upper cover plate of graphite grinding tool are mainly to improve the concentricity after product component freezes.
(4) table top acid corrosion is corroded.The assembled naked diode that will freeze is inserted into dedicated corrosion disk, and uses purity
It is corroded for analytically pure nitric acid, hydrofluoric acid, glacial acetic acid, sulfuric acid mixed acid, configure mixed acid when nitric acid, hydrofluoric acid,
Glacial acetic acid, sulfuric acid volume ratio are 12:9:6:12:;And refrigerate corrosive liquid to 3 DEG C, corrode number three times, 50 seconds every time;Institute
It is respectively as follows: 65%, 40%, 99.5%, 95% with the mass percent concentration of nitric acid, hydrofluoric acid, glacial acetic acid, sulfuric acid, corrodes
The a large amount of deionized waters of Cheng Houyong are rinsed.Above-mentioned mixed acid has preferable corrosiveness with comparison chip, makes chip platform
Face corrosion is bright, can reduce its corrosion to copper lead and molybdenum electrode in electrode material to the greatest extent again simultaneously.
(5) table top caustic corrosion.Product after acid corrosion is cleaned is put into the potassium hydroxide solution of concentration 3%, solution temperature
90 DEG C, etching time 3min of degree is rinsed after taking-up with a large amount of hot and cold deionized waters, number 10 times, and the purpose of caustic corrosion is to remove
The metal and foreign ion of chip table are attached to after acid corrosion.Form more clean table top.
(6) Passivation Treatment, after caustic corrosion is cleaned volume product carry out thermal inactivation processing, passivating solution proportion be hydrogen peroxide,
Phosphoric acid, deionized water press 2:2:5, and passivating solution temperature is at 55 DEG C, and twice, time 1min, hydrogen peroxide used, phosphoric acid are pure for passivation number
Degree is pure, the mass percent 30%, 85% of analysis.The purpose of thermal inactivation is to grow layer of silicon dioxide in chip surface wet process
Passivation layer, wherein phosphoric acid is mainly buffer solution, provides acid ion, and the effect of hydrogen peroxide is to generate titanium dioxide with pasc reaction
Silicon realizes silicon face passivation protection.Simultaneously because passivating solution is acidic liquid, acidic liquid progress is added in product after caustic corrosion
Passivation has also reached certain neutralization, and the product component after making caustic corrosion is easier to clean up.
(7) encapsulated moulding.Tube core after corrosion cleaning is loaded in graphite bar, using automatic dusting and uniformly on table top
Coating glass slurry forms uniform sphere, and wherein passivation glass powder is specific glass powder, and granularity contains in 800 mesh, glass powder
Lead amount is sent into low temperature moulding furnace after 2%, dusting and is formed, 2 hours of molding time, and 10 DEG C of equipment heating rate/
Min, heating-up time 45min, 660 DEG C of maximum sintering temperature, constant temperature time 5min, 5 DEG C/min of rate of temperature fall.Product through high temperature at
Glass powder paste melts the passivation and encapsulation effect of the chip table of solidifying realization, the glass passivation layer thickness in chip table region after type
1mm。
Embodiment 2:
A kind of highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method, using molybdenum as contact conductor, pipe
For core using aluminium as solder, chip uses depth-diffusion process, and table top moulding is orthogonal rake moulding, which reduces surface
Electric field, while before carrying out glassivation encapsulation, chip table is protected using acid, caustic corrosion technique and passivation technology,
Then high temperature is carried out using specific glass powder and is passivated encapsulated moulding;The specific steps are that:
(1) tube core is prepared.PN junction, then the side for passing through electron beam evaporation are formed on monocrystalline silicon piece by deep method of diffusion of tying
Method, for aluminium or the metal film layer of silver, then is cut by blast in the face P of PN junction and N wheat flour and will be coated with the monocrystalline of metal film layer
The molding of silicon wafer blast becomes the tube core in bucking ladder face.
(2) corrosion cleaning tube core.The tube core of well cutting is carried out using the mixed acid of nitric acid, hydrofluoric acid, sulfuric acid, glacial acetic acid
Corrosion, nitric acid, hydrofluoric acid, sulfuric acid and glacial acetic acid mass percentage concentration be respectively as follows: 66%, 50%, 96%, 99.7% mixed acid
Middle nitric acid, hydrofluoric acid, sulfuric acid and glacial acetic acid volume proportion be 8:2:2:5, etching time 15min, the pipe after etching
Core with acetone carries out ultrasonic cleaning primary, time 10min, in primary, the time 10min that carries out ultrasonic cleaning with alcohol, so
It is dehydrated, dries afterwards.Cleaned by the corrosion of above-mentioned mixed acid, can effectively remove chip table mechanical damage layer and impurity from
Son.
(3) it freezes assembling.Using brazing piece as solder, by high temperature sintering methods by molybdenum or tungsten electrode and copper metal lead
Or welding wire welding lead forms whole contact conductor together, the temperature of high temperature sintering is 850 DEG C;Again by two electrodes
Lead and tube core are with being assembled into graphite jig, graphite grinding tool upper cover plate and lower cover plate, two contact conductors when combo
Electrode end surface is in close contact with the metallic film on the face P and the face N of tube core respectively, and contact conductor, tube core, contact conductor successively erect
It directly stacks, then graphite jig is put into vacuum sintering furnace, and contact conductor and tube core are subjected to melting welding bonding, aluminium at high temperature
The corresponding melting welding bonding temperature of metallic film is 650 DEG C, improves the quality of melting welding bonding.Metallic film on tube core is to realize electricity
The solder that pole lead is bonded with tube core, the upper cover plate of graphite grinding tool are mainly to improve the concentricity after product component freezes.
(4) table top acid corrosion is corroded.The assembled naked diode that will freeze is inserted into dedicated corrosion disk, and uses purity
It is corroded for analytically pure nitric acid, hydrofluoric acid, glacial acetic acid, sulfuric acid mixed acid, configure mixed acid when nitric acid, hydrofluoric acid,
Glacial acetic acid, sulfuric acid volume ratio are 12:9:6:12:;And refrigerate corrosive liquid to 2 DEG C, corrode number three times, 50 seconds every time;Institute
It is respectively as follows: 66%, 50%, 99.6%, 96% with the mass percent concentration of nitric acid, hydrofluoric acid, glacial acetic acid, sulfuric acid, corrodes
The a large amount of deionized waters of Cheng Houyong are rinsed.Above-mentioned mixed acid has preferable corrosiveness with comparison chip, makes chip platform
Face corrosion is bright, can reduce its corrosion to copper lead and molybdenum electrode in electrode material to the greatest extent again simultaneously.
(5) table top caustic corrosion.Product after acid corrosion is cleaned is put into the potassium hydroxide solution of concentration 4%, solution temperature
92 DEG C, etching time 4min of degree is rinsed after taking-up with a large amount of hot and cold deionized waters, number 10 times, and the purpose of caustic corrosion is to remove
The metal and foreign ion of chip table are attached to after acid corrosion.Form more clean table top.
(6) Passivation Treatment, after caustic corrosion is cleaned volume product carry out thermal inactivation processing, passivating solution proportion be hydrogen peroxide,
Phosphoric acid, deionized water press 2:2:5, passivating solution temperature between 59 DEG C, passivation number twice, time 2min, hydrogen peroxide used, phosphorus
Sour purity is to analyze pure, mass percent 50%, 87%.The purpose of thermal inactivation is to grow one layer of dioxy in chip surface wet process
SiClx passivation layer, wherein phosphoric acid is mainly buffer solution, provides acid ion, and the effect of hydrogen peroxide is to generate dioxy with pasc reaction
SiClx realizes silicon face passivation protection.Simultaneously because passivating solution is acidic liquid, product be added after caustic corrosion acidic liquid into
Row passivation has also reached certain neutralization, and the product component after making caustic corrosion is easier to clean up.
(7) encapsulated moulding.Tube core after corrosion cleaning is loaded in graphite bar, using automatic dusting and uniformly on table top
Coating glass slurry forms uniform sphere, and wherein passivation glass powder is specific glass powder, and granularity contains in 900 mesh, glass powder
Lead amount is sent into low temperature moulding furnace after 5%, dusting and is formed, 2.3 hours of molding time, and 12 DEG C of equipment heating rate/
Min, heating-up time 50min, 660 DEG C of maximum sintering temperature, constant temperature time 9min, by warm 4 DEG C/min of rate.Product through high temperature at
Glass powder paste melts the passivation and encapsulation effect of the chip table of solidifying realization, the glass passivation layer thickness in chip table region after type
1.2mm。
Embodiment 3:
A kind of highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method, using tungsten as contact conductor, pipe
For core using aluminium as solder, chip uses depth-diffusion process, and table top moulding is orthogonal rake moulding, which reduces surface
Electric field, while before carrying out glassivation encapsulation, chip table is protected using acid, caustic corrosion technique and passivation technology,
Then high temperature is carried out using specific glass powder and is passivated encapsulated moulding;The specific steps are that:
(1) tube core is prepared.PN junction, then the side for passing through electron beam evaporation are formed on monocrystalline silicon piece by deep method of diffusion of tying
Method, for aluminium or the metal film layer of silver, then is cut by blast in the face P of PN junction and N wheat flour and will be coated with the monocrystalline of metal film layer
The molding of silicon wafer blast becomes the tube core in bucking ladder face.
(2) corrosion cleaning tube core.The tube core of well cutting is carried out using the mixed acid of nitric acid, hydrofluoric acid, sulfuric acid, glacial acetic acid
Corrosion, nitric acid, hydrofluoric acid, sulfuric acid and glacial acetic acid mass percentage concentration be respectively as follows: 67%, 55%, 97%, 99.7% mixed acid
Middle nitric acid, hydrofluoric acid, sulfuric acid and glacial acetic acid volume proportion be 8:2:2:5, etching time 15.5min, after etching
Tube core with acetone carries out ultrasonic cleaning primary, time 10min, in primary, the time 10min that carries out ultrasonic cleaning with alcohol,
Then it is dehydrated, dries.It is cleaned by the corrosion of above-mentioned mixed acid, the mechanical damage layer and impurity of chip table can be effectively removed
Ion.
(3) it freezes assembling.Using brazing piece as solder, by high temperature sintering methods by molybdenum or tungsten electrode and copper metal lead
Or welding wire welding lead forms whole contact conductor together, the temperature of high temperature sintering is 870 DEG C;Again by two electrodes
Lead and tube core are with being assembled into graphite jig, graphite grinding tool upper cover plate and lower cover plate, two contact conductors when combo
Electrode end surface is in close contact with the metallic film on the face P and the face N of tube core respectively, and contact conductor, tube core, contact conductor successively erect
It directly stacks, then graphite jig is put into vacuum sintering furnace, and contact conductor and tube core are subjected to melting welding bonding, aluminium at high temperature
The corresponding melting welding bonding temperature of metallic film is 665 DEG C, improves the quality of melting welding bonding.Metallic film on tube core is to realize electricity
The solder that pole lead is bonded with tube core, the upper cover plate of graphite grinding tool are mainly to improve the concentricity after product component freezes.
(4) table top acid corrosion is corroded.The assembled naked diode that will freeze is inserted into dedicated corrosion disk, and uses purity
It is corroded for analytically pure nitric acid, hydrofluoric acid, glacial acetic acid, sulfuric acid mixed acid, configure mixed acid when nitric acid, hydrofluoric acid,
Glacial acetic acid, sulfuric acid volume ratio are 12:9:6:12:;And refrigerate corrosive liquid to 2.5 DEG C, corrode number three times, 50 seconds every time;
Nitric acid used, hydrofluoric acid, glacial acetic acid, sulfuric acid mass percent concentration be respectively as follows: 67%, 55%, 99.7%, 95%~
98%, it is rinsed after etching with a large amount of deionized waters.Above-mentioned mixed acid with comparison chip there is preferable corrosion to make
With making that chip table top etching is bright, can reduce its corrosion to copper lead and molybdenum electrode in electrode material to the greatest extent again simultaneously.
(5) table top caustic corrosion.Product after acid corrosion is cleaned is put into the potassium hydroxide solution of concentration 5%, solution temperature
94 DEG C, etching time 4min of degree is rinsed after taking-up with a large amount of hot and cold deionized waters, number 10 times, and the purpose of caustic corrosion is to remove
The metal and foreign ion of chip table are attached to after acid corrosion.Form more clean table top.
(6) Passivation Treatment, after caustic corrosion is cleaned volume product carry out thermal inactivation processing, passivating solution proportion be hydrogen peroxide,
Phosphoric acid, deionized water press 2:2:5, passivating solution temperature between 58 DEG C, passivation number twice, time 2.5min, hydrogen peroxide used,
Phosphoric acid purity is to analyze pure, mass percent 60%, 93%.The purpose of thermal inactivation is to grow one layer two in chip surface wet process
Silicon oxide passivation layer, wherein phosphoric acid is mainly buffer solution, provides acid ion, and the effect of hydrogen peroxide is to generate two with pasc reaction
Silica realizes silicon face passivation protection.Simultaneously because passivating solution is acidic liquid, acidic liquid is added in product after caustic corrosion
It is passivated the neutralization for also having reached certain, the product component after making caustic corrosion is easier to clean up.
(7) encapsulated moulding.Tube core after corrosion cleaning is loaded in graphite bar, using automatic dusting and uniformly on table top
Coating glass slurry forms uniform sphere, and wherein passivation glass powder is specific glass powder, and granularity is more than 1000 mesh, glass
Glass powder lead tolerance is sent into low temperature moulding furnace after 9%, dusting and is formed, 2.5 hours of molding time, equipment heating rate
14 DEG C/min, heating-up time 60min, 660 DEG C of maximum sintering temperature, constant temperature time 14min, by warm 2 DEG C/min of rate.Product warp
Glass powder paste melts the passivation and encapsulation effect of the chip table of solidifying realization, the glass passivation layer in chip table region after high-temperature molding
Thickness 1.3mm.
Embodiment 4:
A kind of highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method, using tungsten as contact conductor, pipe
For core using aluminium as solder, chip uses depth-diffusion process, and table top moulding is orthogonal rake moulding, which reduces surface
Electric field, while before carrying out glassivation encapsulation, chip table is protected using acid, caustic corrosion technique and passivation technology,
Then high temperature is carried out using specific glass powder and is passivated encapsulated moulding;The specific steps are that:
(1) tube core is prepared.PN junction, then the side for passing through electron beam evaporation are formed on monocrystalline silicon piece by deep method of diffusion of tying
Method, for aluminium or the metal film layer of silver, then is cut by blast in the face P of PN junction and N wheat flour and will be coated with the monocrystalline of metal film layer
The molding of silicon wafer blast becomes the tube core in bucking ladder face.
(2) corrosion cleaning tube core.The tube core of well cutting is carried out using the mixed acid of nitric acid, hydrofluoric acid, sulfuric acid, glacial acetic acid
Corrosion, nitric acid, hydrofluoric acid, sulfuric acid and glacial acetic acid mass percentage concentration be respectively as follows: 68%, 60%, 98%, 99.8% mixed acid
Middle nitric acid, hydrofluoric acid, sulfuric acid and glacial acetic acid volume proportion be 8:2:2:5, etching time 16min, the pipe after etching
Core with acetone carries out ultrasonic cleaning primary, time 10min, in primary, the time 10min that carries out ultrasonic cleaning with alcohol, so
It is dehydrated, dries afterwards.Cleaned by the corrosion of above-mentioned mixed acid, can effectively remove chip table mechanical damage layer and impurity from
Son.
(3) it freezes assembling.Using brazing piece as solder, by high temperature sintering methods by molybdenum or tungsten electrode and copper metal lead
Or welding wire welding lead forms whole contact conductor together, the temperature of high temperature sintering is 900 DEG C;Again by two electrodes
Lead and tube core are with being assembled into graphite jig, graphite grinding tool upper cover plate and lower cover plate, two contact conductors when combo
Electrode end surface is in close contact with the metallic film on the face P and the face N of tube core respectively, and contact conductor, tube core, contact conductor successively erect
It directly stacks, then graphite jig is put into vacuum sintering furnace, and contact conductor and tube core are subjected to melting welding bonding, aluminium at high temperature
The corresponding melting welding bonding temperature of metallic film is 680 DEG C, improves the quality of melting welding bonding.Metallic film on tube core is to realize electricity
The solder that pole lead is bonded with tube core, the upper cover plate of graphite grinding tool are mainly to improve the concentricity after product component freezes.
(4) table top acid corrosion is corroded.The assembled naked diode that will freeze is inserted into dedicated corrosion disk, and uses purity
It is corroded for analytically pure nitric acid, hydrofluoric acid, glacial acetic acid, sulfuric acid mixed acid, configure mixed acid when nitric acid, hydrofluoric acid,
Glacial acetic acid, sulfuric acid volume ratio are 12:9:6:12:;And refrigerate corrosive liquid to 2.5 DEG C, corrode number three times, 50 seconds every time;
Nitric acid used, hydrofluoric acid, glacial acetic acid, sulfuric acid mass percent concentration be respectively as follows: 68%, 60%, 99.8%, 98%, corrosion
It is rinsed after the completion with a large amount of deionized waters.Above-mentioned mixed acid has preferable corrosiveness with comparison chip, makes chip
Mesa etch is bright, can reduce its corrosion to copper lead and molybdenum electrode in electrode material to the greatest extent again simultaneously.
(5) table top caustic corrosion.Product after acid corrosion is cleaned is put into the potassium hydroxide solution of concentration 6%, solution temperature
95 DEG C, etching time 5min of degree is rinsed after taking-up with a large amount of hot and cold deionized waters, number 10 times, and the purpose of caustic corrosion is to remove
The metal and foreign ion of chip table are attached to after acid corrosion.Form more clean table top.
(6) Passivation Treatment, after caustic corrosion is cleaned volume product carry out thermal inactivation processing, passivating solution proportion be hydrogen peroxide,
Phosphoric acid, deionized water press 2:2:5, passivating solution temperature between 58 DEG C, passivation number twice, time 2.5min, hydrogen peroxide used,
Phosphoric acid purity is to analyze pure, mass percent 65%, 95%.The purpose of thermal inactivation is to grow one layer two in chip surface wet process
Silicon oxide passivation layer, wherein phosphoric acid is mainly buffer solution, provides acid ion, and the effect of hydrogen peroxide is to generate two with pasc reaction
Silica realizes silicon face passivation protection.Simultaneously because passivating solution is acidic liquid, acidic liquid is added in product after caustic corrosion
It is passivated the neutralization for also having reached certain, the product component after making caustic corrosion is easier to clean up.
(7) encapsulated moulding.Tube core after corrosion cleaning is loaded in graphite bar, using automatic dusting and uniformly on table top
Coating glass slurry forms uniform sphere, and wherein passivation glass powder is specific glass powder, and granularity is more than 1200 mesh, glass
Glass powder lead tolerance is sent into low temperature moulding furnace after 10%, dusting and is formed, 3 hours of molding time, equipment heating rate
15 DEG C/min, heating-up time 65min, 660 DEG C of maximum sintering temperature, constant temperature time 15min, by warm 1.5 DEG C/min of rate.Product
Glass powder paste melts the passivation and encapsulation effect of the chip table of solidifying realization, the glassivation in chip table region after high-temperature molding
Thickness degree 1.4mm.
Claims (9)
1. a kind of highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method, using molybdenum or tungsten as contact conductor,
For tube core using aluminium as solder, chip uses depth-diffusion process, and table top moulding is orthogonal rake moulding, which reduces table
Face electric field, while before carrying out glassivation encapsulation, chip table is protected using acid, caustic corrosion technique and passivation technology
Then shield carries out high temperature using specific glass powder and is passivated encapsulated moulding;The specific steps are that:
A) PN junction is formed on monocrystalline silicon piece by deep method of diffusion of tying, then passes through the method for electron beam evaporation in the face P of PN junction
With N wheat flour for aluminium or the metal film layer of silver;
B) it is cut by blast and the monocrystalline silicon piece blast for being coated with metal film layer is molded into the tube core that section is trapezoidal table top;
C) corrosion 14~16min of cleaning is carried out to the tube core of well cutting using cleaning agent, tube core acetone after etching into
Row 8~12min of ultrasonic cleaning, then 8~12min of ultrasonic cleaning is carried out with alcohol, it is then dehydrated, dries;
D) electrode and metal lead wire freeze into the contact conductor of an entirety by high temperature sintering, then by contact conductor, tube core,
Contact conductor is successively vertically stacked in graphite jig, then graphite jig is put into contact conductor and tube core in vacuum sintering furnace
Carry out melting welding key and;
E) it is corroded using acid corrosion liquid in the diode insertion corrosion disk after freezing, ion is used after etching
Water cleaning;
F) diode after acid corrosion is put into 3~5min of corrosion cleaning in caustic corrosion liquid, is handed over after removal with hot and cold deionized water
For flushing 10 times;
G) diode after acid corrosion, which is put into the passivating solution that temperature is 55~60 DEG C, is passivated 1~3min;
H) diode after passivation is loaded in graphite bar, using automatic dusting and uniform coated particle degree 800 on table top
Glass powder paste more than mesh forms uniform sphere, is sent into low temperature moulding furnace after dusting and carries out 2~3h of molding.
2. highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method as described in claim 1, it is characterised in that:
The cleaning agent be by mass percentage 65%~68% nitric acid, >=40% hydrofluoric acid, 95%~98% sulfuric acid, >=
The mixed solution of 99.5% glacial acetic acid 8:2:2:5 by volume.
3. highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method as described in claim 1, it is characterised in that:
The solder of the high temperature sintering is brazing piece, and high temperature sintering temperature is 800~900 DEG C.
4. highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method as described in claim 1, it is characterised in that:
Metallic film on the tube core is the solder of tube core key sum, and the temperature of melting welding key sum is 620~750 DEG C.
5. highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method as described in claim 1, it is characterised in that:
The acid corrosion liquid is analytically pure 65%~68% nitric acid, >=40% hydrofluoric acid, 95%~98% by mass percentage
Sulfuric acid, >=99.5% glacial acetic acid 12:9:12:6 by volume mixed solution.
6. highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method as described in claim 1, it is characterised in that:
The potassium hydroxide solution that the caustic corrosion liquid is 3%~6%, caustic corrosion liquid temperature are 90~95 DEG C.
7. highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method as described in claim 1, it is characterised in that:
The passivating solution be by mass percentage >=30% hydrogen peroxide, >=85% hydrogen peroxide and ionized water mixed by 2:2:5 it is mixed
Close liquid.
8. highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method as described in claim 1, it is characterised in that:
In the glass powder containing 2%~10% lead, the coefficient of expansion is close with molybdenum, tungsten electrode.
9. highly reliable Flouride-resistani acid phesphatase glassivation voltage adjustment diode manufacturing method as described in claim 1, it is characterised in that:
The low temperature moulding furnace heating rate 10~15 DEG C/min, 45~65min of heating-up time, 660 DEG C of maximum sintering temperature, when constant temperature
Between 5~15min, rate of temperature fall≤5 DEG C/min.
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CN107393822A (en) * | 2017-07-17 | 2017-11-24 | 中国振华集团永光电子有限公司(国营第八七三厂) | A kind of manufacture method suppressed with transient voltage with the glassivation fly-wheel diode of rectification function |
CN108447768A (en) * | 2018-01-25 | 2018-08-24 | 如皋市远亚电子有限公司 | A kind of production technology of OJ chip manufacturings diode |
CN110970298B (en) * | 2019-12-30 | 2023-08-04 | 中国振华集团永光电子有限公司(国营第八七三厂) | Epoxy packaged micro diode and manufacturing process thereof |
CN111180312B (en) * | 2019-12-31 | 2023-08-11 | 贵州振华风光半导体股份有限公司 | Reflow soldering cleaning method suitable for integrated circuit |
CN113290217B (en) * | 2021-05-28 | 2022-09-23 | 金川集团股份有限公司 | Vacuum continuous casting process of high-purity oxygen-free copper rod |
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