CN109459476A - A kind of all-solid-state reference electrode Preparation equipment and its method based on EB-PVD and SOL-GEL - Google Patents
A kind of all-solid-state reference electrode Preparation equipment and its method based on EB-PVD and SOL-GEL Download PDFInfo
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- CN109459476A CN109459476A CN201811654516.2A CN201811654516A CN109459476A CN 109459476 A CN109459476 A CN 109459476A CN 201811654516 A CN201811654516 A CN 201811654516A CN 109459476 A CN109459476 A CN 109459476A
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- G01N27/28—Electrolytic cell components
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- G01N27/301—Reference electrodes
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Abstract
The invention discloses a kind of all-solid-state reference electrode Preparation equipments based on EB-PVD and SOL-GEL, it is related to motor and prepares correlative technology field, including agitating device and solidification room, the upper surface of the agitating device is fixedly connected with feed inlet, the inside of the agitating device offers feeding-passage, the feeding-passage is located at the lower section of feed inlet, and the feed inlet and feeding-passage are interconnected, and the bottom of the feeding-passage offers stirred tank.The invention also discloses a kind of all-solid-state reference electrode preparation methods based on EB-PVD and SOL-GEL, including A: deposition, B: mixing, C: stirring, D: compacting, E: addition, F: drying, G: cooling, H: filling, I: encapsulation saves.Stirring material can be placed in the inside of agitating device by feed inlet by the present invention, and the inside of stirred tank is entered by feeding-passage, and servo motor drives second gear to rotate by shaft, and first gear is bevel gear.
Description
Technical field
It is the present invention relates to electrode preparation apparatus correlative technology field, in particular to a kind of based on EB-PVD's and SOL-GEL
All-solid-state reference electrode Preparation equipment and its method.
Background technique
YSZ solid electrolyte is the high temperature oxygen ion conductor studied and be most widely used, the electrochemical cell being made of it
It is largely used to the on-line checking of oxygen, carbon dioxide, methane and other volatile components, for YSZ solid electrolyte two
Aoxidize carbon sensor, usually using the LizCO with carbon dioxide sensitivity characteristic: and based on the compound carbonate of LizCO3 as
Its key structure of sensitive electrode material LizCO3/YSZ electrode system as such sensor.
Steel and concrete structure is now and one of the primary structure pattern that will be used in considerable time later reinforcement corrosion
It is the main reason for reducing steel and concrete structure durability and causing heavy losses, the harm of reinforcement corrosion is big unexpectedly, with
The deterioration of global climate and environment, this problem outlet increasingly acute situation, steel and concrete structure corrosion of reinforcing steel bar certainly will be presented
Just causing whole world extensive concern.
The corrosion monitoring system based on electrochemical techniques is established, the etch state of reinforcing bar can in real time, be accurately grasped, be big
The safety evaluation of scale steel and concrete structure and full-time design provide scientific basis.The electro-chemical test skill of corrosion sensor horn of plenty
Art provides hardware supported, is to ensure that various corrosion monitoring process can be able to the carrier applied and platform in practical projects.
In Chinese invention patent application number: disclosing a kind of electrode preparation method in 107976474 A of CN, a kind of electricity
Pole preparation method, although electrode can be prepared by this method, the efficiency that this method produces the electrode is lower, electrode it is steady
It is qualitative not strong and inconvenient by step production electrode, the production efficiency of electrode is influenced, the production efficiency of electrode is reduced.
It is therefore proposed that a kind of solved based on the all-solid-state reference electrode Preparation equipment of EB-PVD and SOL-GEL and its method
Certainly the above problem is necessary.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of, and all solid state reference based on EB-PVD and SOL-GEL is electric
Pole Preparation equipment and its method, solve in current electrode preparation that production efficiency is low, the problem of the electrode stability difference of production.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of all-solid-state reference electrode Preparation equipment based on EB-PVD and SOL-GEL, comprising:
Agitating device and solidification room, the upper surface of the agitating device are fixedly connected with feed inlet, the agitating device
Inside offers feeding-passage, and the feeding-passage is located at the lower section of feed inlet, and the feed inlet and feeding-passage are interconnected；
The bottom of the feeding-passage offers stirred tank, and the inside of the agitating device is opened far from the side of feeding-passage
Equipped with the first rotation slot, the internal activity of first rotation slot is connected with first gear, and the side of first rotation slot is opened
Equipped with the second rotation slot, the internal activity of second rotation slot is connected with second gear, a middle side part of the second gear
It is fixedly connected with shaft, the shaft sequentially passes through side and the agitating device of the second rotation slot far from one end of second gear
Side and the outside for being located at agitating device；
Connecting shaft, the one end of the connecting shaft far from first gear are fixedly connected in the middle part of the lower surface of the first gear
Through stirred tank upper surface middle part and be located at the inside of stirred tank, be fixedly connected in the bottom circumferential direction of the connecting shaft multiple
Paddle；
Transmission channel is offered in the middle part of the lower surface of the stirred tank, the internal activity of the transmission channel is equipped with connection
Bar is fixedly connected with sprue at the top of the connecting rod, and the side of the transmission channel offers control flume, the connecting rod
Bottom side is fixedly connected with control-rod, and the control-rod runs through the side of control flume far from one end of connecting rod and is located at control
The inside of slot；
The inside of the control flume is fixedly installed with articulation piece, and the middle part of the control-rod is flexibly connected with articulation piece, institute
The inside that control-rod is movably arranged on control flume by articulation piece is stated, the upper surface of the control-rod is solid far from the side of connecting rod
Surely it is connected with spring, the spring is fixedly connected on the upper surface side of control flume far from one end of control-rod；
The lower surface of the agitating device is fixedly connected with connecting tube, and the bottom of the connecting tube is fixedly connected with solidification
Room, the transmission channel and connecting tube are interconnected；
The one end of the connecting tube far from agitating device is through the upper surface middle part for solidifying room and is fixedly connected with isocon,
One end of the connecting tube is fixedly connected with the upper surface middle part of isocon, and the lower surface of the isocon is fixedly connected with multiple
Branch pipe is fixedly installed with support plate in the middle part of the solidification room, and the upper surface of the support plate is fixedly installed with multiple coagulating basins,
Drying oven is fixedly installed in the middle part of the lower surface of the solidification room.
Optionally, the stirred tank is in bucket type structure, is adapted in the middle part of the sprue and the lower surface of stirred tank, described stifled
Inside of the top of block in the middle part of the lower surface of stirred tank and positioned at stirred tank.
Optionally, the quantity of the paddle is no less than three, two neighboring paddle spaced set, the paddle
Middle part offer opening.
Optionally, the shaft runs through the top side of agitating device far from one end of second gear, and the shaft is located at
One end outside agitating device is connected with servo motor.
Optionally, first rotation slot is mutually perpendicular to the second rotation slot, first rotation slot and the second rotation slot
It is interconnected, the first gear is bevel gear, and company is engaged with the side of second gear in the upper surface side of the first gear
It connects.
Optionally, the arms parallel is distributed in the lower surface of isocon, and the distance between two neighboring branch pipe is equal.
The upper surface of the solidification room offers multiple drying holes, and the drying hole is in as the center of circle using the central point for solidifying room
Annular array distribution.
A method of the all-solid-state reference electrode preparation based on EB-PVD and SOL-GEL, comprising the following steps:
A: deposition: by EP-PVD technology, deposition obtains bianry alloy film from Ti stick matrix, and the binary of acquirement is closed
The Ti stick of gold thin film, which is placed in high temperature furnace, carries out oxidation processes, and oxidizing temperature is 600 DEG C~800 DEG C, and oxidization time is 8~
10min, the heating rate in high temperature furnace are 10 DEG C~15 DEG C/min；
B: mixing: by active material powder, conductive agent powder, binder powder according to 30~100: 2~10: 5~15
Ratio is stirred；
C: stirring: mixed powder is put into blender by funnel, blender is with the stirring rate of 500~800/min
Mixed powder is stirred evenly, mixing time is 10~20min；
D: compacting: the mixed powder after stirring is pressed into dry film, is then compressed on dry film by hot pressing complex method
The inside of Ti stick, and encapsulated holes are reserved at the center of Ti stick, the compound temperature range of hot pressing is 80 DEG C~130 DEG C,；
E: addition: mixing merga pass blender for acrylamide and acrylic acid with 1: 1 ratio and stir evenly, acrylamide
The 40%~60% of function core gross mass is accounted for acrylic acid, then by mixed gel agent and methylene-bisacrylamide with 1: 2
Ratio is mixed merga pass blender and is stirred evenly, and mixed gel agent and methylene-bisacrylamide account for function core gross mass
30%~50%, the potassium chloride that concentration is 1~3M is then added in blender and stirs evenly, potassium chloride accounts for the new gross mass of function
2%, finally tetrafluoro boric acid and hydrogen peroxide will be added again with 1: 1 ratio in mixture, and stir evenly by blender,
The ratio of tetrafluoro boric acid and hydrogen peroxide accounts for the 10% of function core gross mass；
F: drying: mixing material is reacted into the concentration mixed and is stored by distilling box, is then placed in baking vessel
Oven on be dehydrated, baking time be 30~50min, toast indoor temperature be 140~170 DEG C, it is dense after baking
Contracting reaction mixing material forms gelinite；
G: cooling: gelinite being taken out out of baking vessel, the gelinite of high-temperature process is stood, the temperature of high temperature gel body is made
Degree is down to room temperature；
H: filling: in the interior welds copper conductor of the encapsulated holes of Ti stick, while in the uniform gel filled body in the outside of Ti stick,
Gelinite is wrapped up by PVC shell, after gelinite filling, PVC shell is screwed into fastening；
I: encapsulation saves: the quality in order to guarantee the function core, after PVC shell screws fastening, by medical sponge to function
Energy core is wrapped up and is placed in vacuum box, is opened vacuum box when need to use and is needed immediately to make function core
With.
Optionally, in the step B, temperature range is 50~70 DEG C before active material powder mixes, and conductive agent powder is mixed
Temperature range is 60 DEG C~80 DEG C before closing, and temperature range is 80 DEG C~100 DEG C before binder powder mixes.
Optionally, in the step E, acrylamide and acrylic acid are mixed in proportion first, by blender with 700~
The rate of 800r/min is stirred, and mixing time is 6~10min, then by mixed gel agent and methylene bisacrylamide acyl
Amine mix with material is mixed, and is stirred evenly by blender with the rate of 700~800r/min, mixing time for 8~
15min, then potassium chloride is mixed with material is mixed, it is stirred evenly, is stirred with the rate of 700~800r/min by blender
Mixing the time is 3~5min, finally mixes tetrafluoro boric acid and hydrogen peroxide with mixing material, by blender with 700~
The rate of 800r/min stirs evenly, and mixing time is 4~7min.
Optionally, it in the step F, toasts indoor temperature and is heated up with the speed of 10 DEG C/min.
(3) beneficial effect
The present invention provides a kind of all-solid-state reference electrode Preparation equipment and its method based on EB-PVD and SOL-GEL,
Have it is following the utility model has the advantages that
(1), stirring material can be placed in the inside of agitating device by feed inlet by the present invention, entered by feeding-passage and stirred
The inside of slot is mixed, servo motor drives second gear to rotate by shaft, and first gear is bevel gear, and second gear passes through first
Gear drives paddle to be rotated, and carries out uniform stirring to the material in stirred tank, is driven by servo motor more automatic
Change, not only time saving and energy saving but also smaller to the abrasion of servo motor, service life is higher, passes through control-rod, articulation piece and spring
Setting, using articulation piece as fulcrum, the other end of control-rod is made to drive sprue to moving down by one end of upward lift control bar
Dynamic, entering the material in stirred tank after stirring by transmission channel, solidification is indoor, and passes through the shunting of solidification chamber interior setting
Material after stirring is respectively implanted the inside of coagulating basin by pipe and branch pipe, carries out drying solidification to material by drying oven, is applicable in
Range is more extensive, and production efficiency is higher
(2), the present invention is mixed by active material powder, conductive agent powder and binder powder, then repressed equipment
Mixed powder is compressed on to the inside of Ti stick, electric current is conducted by copper conductor and mixed powder, passes through mixed powder and Ti stick
The inner core of motor is made, concentration reaction mixing material is then formed into gelinite by oven dewatered drying, then by gel
Body is uniformly wrapped in the outer surface of Ti stick, then gelinite is fixed by PVC shell, makes the total quality of the function core more
Height, when use, are more stable.
Detailed description of the invention
Fig. 1 is agitating device schematic structural cross-sectional view of the invention；
Fig. 2 is solidification cell structure schematic cross-sectional view of the invention；
Fig. 3 is stirring impeller structure schematic top plan view of the invention；
Fig. 4 is solidification cell structure schematic top plan view of the invention.
In figure: 1- agitating device, 2- solidify room, 3- feed inlet, 4- feeding-passage, 5- stirred tank, the first rotation slot of 6-, 7-
First gear, the second rotation slot of 8-, 9- second gear, 10- shaft, 11- connecting shaft, 12- paddle, 13- transmission channel, 14-
Connecting rod, 15- sprue, 16- control-rod, 17- control flume, 18- spring, 19- articulation piece, 20- connecting tube, 21- isocon, 22-
Branch pipe, 23- support plate, 24- coagulating basin, 25- drying oven, 26- drying hole.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that, term " center ", " length " "upper", "lower", "front", "rear",
The orientation or positional relationship of the instructions such as "horizontal", "top", "bottom" "inner", "outside", " circumferential direction " be orientation based on the figure or
Positional relationship is merely for convenience of description of the present invention and simplification of the description, rather than the device or element of indication or suggestion meaning must
There must be specific orientation, be constructed and operated in a specific orientation, therefore be not considered as limiting the invention.
In the present invention unless specifically defined or limited otherwise, term " setting ", " installation ", " connected ", " connection ",
Terms such as " fixations " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection；It can be mechanical connect
It connects；It can be directly connected, it can also be indirectly connected through an intermediary.For the ordinary skill in the art, may be used
To understand the concrete meaning of above-mentioned term in the present invention as the case may be.
In addition, term " first ", " second " etc. are used for description purposes only, it is not understood to indicate or imply relatively important
Property or implicitly indicate the quantity of indicated technical characteristic.Define " first " as a result, the feature of " second " can be expressed or
Person implicitly includes one or more of the features.
According to a kind of technical solution as shown in Figs 1-4, that the present invention has supplied:
A kind of all-solid-state reference electrode Preparation equipment based on EB-PVD and SOL-GEL, comprising:
Agitating device 1 and solidification room 2, the upper surface of agitating device 1 is fixedly connected with feed inlet 3, the inside of agitating device 1
Feeding-passage 4 is offered, feeding-passage 4 is located at the lower section of feed inlet 3, and feed inlet 3 and feeding-passage 4 are interconnected；
The bottom of feeding-passage 4 offers stirred tank 5, and the inside of agitating device 1 is offered far from the side of feeding-passage 4
First rotation slot 6, the internal activity of the first rotation slot 6 are connected with first gear 7, and the side of the first rotation slot 6 offers second
Rotation slot 8, the internal activity of the second rotation slot 8 are connected with second gear 9, and a middle side part of second gear 9, which is fixedly connected with, to be turned
Axis 10, shaft 10 sequentially pass through the side of the second rotation slot 8 and side and the position of agitating device 1 far from one end of second gear 9
In the outside of agitating device 1；
It is fixedly connected with connecting shaft 11 in the middle part of the lower surface of first gear 7, connecting shaft 11 is passed through far from one end of first gear 7
It wears the upper surface middle part of stirred tank 5 and is located at the inside of stirred tank 5, be fixedly connected with multiple stir in the bottom circumferential direction of connecting shaft 11
Mix leaf 12；
Transmission channel 13 is offered in the middle part of the lower surface of stirred tank 5, the internal activity of transmission channel 13 is equipped with connecting rod
14, the top of connecting rod 14 is fixedly connected with sprue 15, and the side of transmission channel 13 offers control flume 17, the bottom of connecting rod 14
Portion side is fixedly connected with control-rod 16, and control-rod 16 runs through the side of control flume 17 far from one end of connecting rod 14 and is located at control
The inside of slot 17 processed；
The inside of control flume 17 is fixedly installed with articulation piece 19, and the middle part of control-rod 16 is flexibly connected with articulation piece 19, control
Bar 16 processed is movably arranged on the inside of control flume 17 by articulation piece 19, and the upper surface of control-rod 16 is far from the side of connecting rod 14
It is fixedly connected with spring 18, spring 18 is fixedly connected on the upper surface side of control flume 17 far from one end of control-rod 16；
The lower surface of agitating device 1 is fixedly connected with connecting tube 20, and the bottom of connecting tube 20 is fixedly connected with solidification room 2,
Transmission channel 13 and connecting tube 20 are interconnected；
The one end of connecting tube 20 far from agitating device 1 is through the upper surface middle part for solidifying room 2 and is fixedly connected with isocon
21, one end of connecting tube 20 is fixedly connected with the upper surface middle part of isocon 21, and the lower surface of isocon 21 is fixedly connected with more
The middle part of a branch pipe 22, solidification room 2 is fixedly installed with support plate 23, and the upper surface of support plate 23 is fixedly installed with multiple coagulating basins
24, it solidifies and is fixedly installed with drying oven 25 in the middle part of the lower surface of room 2.
As a kind of optional technical solution of the invention: stirred tank 5 is in bucket type structure, the following table of sprue 15 and stirred tank 5
Middle face is adapted, inside of the top of sprue 15 in the middle part of the lower surface of stirred tank 5 and positioned at stirred tank 5.
As a kind of optional technical solution of the invention: the quantity of paddle 12 is no less than three, two neighboring paddle
12 spaced sets, the middle part of paddle 12 offer opening, keep stirring efficiency higher by three paddles 12.
As a kind of optional technical solution of the invention: the one end of shaft 10 far from second gear 9 is through agitating device 1
Top side, one end that shaft 10 is located at outside agitating device 1 are connected with servo motor, drive the second tooth by servo motor
Wheel 9 and first gear 7 are rotated, more convenient.
As a kind of optional technical solution of the invention: the first rotation slot 6 is mutually perpendicular to the second rotation slot 8, and first turn
Dynamic slot 6 and the second rotation slot 8 are interconnected, and first gear 7 is bevel gear, the upper surface side of first gear 7 and second gear 9
Side engage connection, by setting bevel gear for first gear 7, first gear 7 while rotating second gear 9 vertically
It can lateral rotation.
As a kind of optional technical solution of the invention: branch pipe 22 is distributed parallelly on the lower surface of isocon 21, and adjacent two
The distance between a branch pipe 22 is equal, and the material for needing to dry is placed in by 22 Duis of branch pipe the inside of coagulating basin 24, is effectively mentioned
High efficiency.
The upper surface of solidification room 2 offers multiple drying holes 26, and drying hole 26 is the center of circle in ring using the central point for solidifying room 2
Shape array distribution makes material drying efficiency in coagulating basin 24 faster by the way that drying hole 26 is arranged.
Working principle: at work, the material for needing to stir is placed in the inside of agitating device 1 by feed inlet 3, is passed through
Feeding-passage 4 can enter the inside of stirred tank 5, open the switch of servo motor, and servo motor drives second gear 9 by shaft
Rotation, first gear 8 are bevel gear, and second gear 9 engages connection with first gear 8, pass through the rotation drive of second gear 9 the
One gear 8 is rotated, so that paddle 12 be driven to be rotated, is carried out by paddle 12 to the material in stirred tank 5 equal
Even stirring, stirred tank 5 are bucket type structure, and the material after stirring can be gathered to the middle part of stirred tank 5, if material needs at drying
Reason, by one end of upward lift control bar 16, with articulation piece 19 be fulcrum make control-rod 16 the other end drive sprue 15 to
Lower movement enters the material after stirring in stirred tank 5 in solidification room 2 by transmission channel 13, then by solidifying inside room 2
Material after stirring is respectively implanted the inside of coagulating basin 24 by the isocon 21 and branch pipe 22 of setting, by drying oven 25 to material
Carry out drying solidification.
Embodiment one:
A method of the all-solid-state reference electrode preparation based on EB-PVD and SOL-GEL, which is characterized in that including following
Step:
A: deposition: by EP-PVD technology, deposition obtains bianry alloy film from Ti stick matrix, and the binary of acquirement is closed
The Ti stick of gold thin film, which is placed in high temperature furnace, carries out oxidation processes, and oxidizing temperature is 600 DEG C, oxidization time 8min, high temperature furnace
Interior heating rate is 10 DEG C/min；
B: mixing: active material powder, conductive agent powder, binder powder are stirred according to 30: 2: 5 ratio；
C: stirring: mixed powder is put into blender by funnel, blender is with the stirring rate of 500min to mixing
Powder stirring is uniform, mixing time 10min；
D: compacting: the mixed powder after stirring is pressed into dry film, is then compressed on dry film by hot pressing complex method
The inside of Ti stick, and encapsulated holes are reserved at the center of Ti stick, the compound temperature range of hot pressing is 80 DEG C；
E: addition: mixing merga pass blender for acrylamide and acrylic acid with 1: 1 ratio and stir evenly, acrylamide
The 40% of function core gross mass is accounted for acrylic acid, then mixed gel agent and methylene-bisacrylamide is mixed with 1: 2 ratio
Merga pass blender stirs evenly, and mixed gel agent and methylene-bisacrylamide account for the 48% of function core gross mass, so
The potassium chloride that concentration is 1~3M is added in blender afterwards to stir evenly, potassium chloride accounts for the 2% of the new gross mass of function, finally again
Tetrafluoro boric acid and hydrogen peroxide will be added with 1: 1 ratio in mixture, and is stirred evenly by blender, tetrafluoro boric acid and mistake
The ratio of hydrogen oxide accounts for the 10% of function core gross mass；
F: drying: mixing material is reacted into the concentration mixed and is stored by distilling box, is then placed in baking vessel
Oven on be dehydrated, baking time 30min, toasting indoor temperature is 140 DEG C, and mixing is reacted in concentration after baking
Material forms gelinite；
G: cooling: gelinite being taken out out of baking vessel, the gelinite of high-temperature process is stood, the temperature of high temperature gel body is made
Degree is down to room temperature；
H: filling: in the interior welds copper conductor of the encapsulated holes of Ti stick, while in the uniform gel filled body in the outside of Ti stick,
Gelinite is wrapped up by PVC shell, after gelinite filling, PVC shell is screwed into fastening；
I: encapsulation saves: the quality in order to guarantee the function core, after PVC shell screws fastening, by medical sponge to function
Energy core is wrapped up and is placed in vacuum box, is opened vacuum box when need to use and is needed immediately to make function core
With.
As a kind of optional technical solution of the invention: in step B, temperature range is 50 before active material powder mixes
DEG C, temperature range is 60 DEG C before conductive agent powder mixes, and temperature range is 80 DEG C before binder powder mixes.
As a kind of optional technical solution of the invention: in step E, first mixing acrylamide and acrylic acid in proportion
It closes, is stirred by blender with the rate of 700r/min, mixing time 6min, then by mixed gel agent and methylene
Base bisacrylamide is mixed with material is mixed, and is stirred evenly by blender with the rate of 700r/min, mixing time is
8min, then potassium chloride is mixed with material is mixed, it is stirred evenly by blender with the rate of 700r/min, mixing time
For 3min, finally tetrafluoro boric acid and hydrogen peroxide are mixed with material is mixed, by blender with the rate of 700r/min
It stirs evenly, mixing time 4min.
As a kind of optional technical solution of the invention: in step F, toasting indoor temperature with the speed liter of 10 DEG C/min
Temperature
Embodiment two:
A method of the all-solid-state reference electrode preparation based on EB-PVD and SOL-GEL, which is characterized in that including following
Step:
A: deposition: by EP-PVD technology, deposition obtains bianry alloy film from Ti stick matrix, and the binary of acquirement is closed
The Ti stick of gold thin film, which is placed in high temperature furnace, carries out oxidation processes, and oxidizing temperature is 800 DEG C, oxidization time 10min, high temperature furnace
Interior heating rate is 15 DEG C/min；
B: mixing: active material powder, conductive agent powder, binder powder are stirred according to 70: 10: 10 ratio and is mixed
It closes；
Step C: stirring: mixed powder is put into blender by funnel, blender is with the stirring rate pair of 800/min
Mixed powder stirs evenly, mixing time 20min；
D: compacting: the mixed powder after stirring is pressed into dry film, is then compressed on dry film by hot pressing complex method
The inside of Ti stick, and encapsulated holes are reserved at the center of Ti stick, the compound temperature range of hot pressing is 130 DEG C,；
E: addition: mixing merga pass blender for acrylamide and acrylic acid with 1: 1 ratio and stir evenly, acrylamide
The 43% of function core gross mass is accounted for acrylic acid, then mixed gel agent and methylene-bisacrylamide is mixed with 1: 2 ratio
Merga pass blender stirs evenly, and mixed gel agent and methylene-bisacrylamide account for the 45% of function core gross mass, so
The potassium chloride that concentration is 1~3M is added in blender afterwards to stir evenly, potassium chloride accounts for the 2% of the new gross mass of function, finally again
Tetrafluoro boric acid and hydrogen peroxide will be added with 1: 1 ratio in mixture, and is stirred evenly by blender, tetrafluoro boric acid and mistake
The ratio of hydrogen oxide accounts for the 10% of function core gross mass；
F: drying: mixing material is reacted into the concentration mixed and is stored by distilling box, is then placed in baking vessel
Oven on be dehydrated, baking time 50min, toasting indoor temperature is 170 DEG C, and mixing is reacted in concentration after baking
Material forms gelinite；
G: cooling: gelinite being taken out out of baking vessel, the gelinite of high-temperature process is stood, the temperature of high temperature gel body is made
Degree is down to room temperature；
H: filling: in the interior welds copper conductor of the encapsulated holes of Ti stick, while in the uniform gel filled body in the outside of Ti stick,
Gelinite is wrapped up by PVC shell, after gelinite filling, PVC shell is screwed into fastening；
I: encapsulation saves: the quality in order to guarantee the function core, after PVC shell screws fastening, by medical sponge to function
Energy core is wrapped up and is placed in vacuum box, is opened vacuum box when need to use and is needed immediately to make function core
With.
As a kind of optional technical solution of the invention: in step B, temperature range is 70 before active material powder mixes
DEG C, temperature range is 80 DEG C before conductive agent powder mixes, and temperature range is 100 DEG C before binder powder mixes.
As a kind of optional technical solution of the invention: in step E, first mixing acrylamide and acrylic acid in proportion
It closes, is stirred by blender with the rate of 800r/min, mixing time 10min, then by mixed gel agent and Asia
Bisacrylamide is mixed with material is mixed, and is stirred evenly by blender with the rate of 800r/min, mixing time
For 15min, then potassium chloride mix with material is mixed, is stirred evenly by blender with the rate of 800r/min, stirring
Time is 5min, is finally mixed tetrafluoro boric acid and hydrogen peroxide with material is mixed, by blender with 800r/min's
Rate stirs evenly, mixing time 7min.
As a kind of optional technical solution of the invention: in step F, toasting indoor temperature with the speed liter of 10 DEG C/min
Temperature.
Embodiment three:
A method of the all-solid-state reference electrode preparation based on EB-PVD and SOL-GEL, which is characterized in that including following
Step:
A: deposition: by EP-PVD technology, deposition obtains bianry alloy film from Ti stick matrix, and the binary of acquirement is closed
The Ti stick of gold thin film, which is placed in high temperature furnace, carries out oxidation processes, and oxidizing temperature is 700 DEG C, oxidization time 9min, high temperature furnace
Interior heating rate is 13 DEG C/min；
B: mixing: active material powder, conductive agent powder, binder powder are stirred according to 50: 7: 12 ratio；
C: stirring: mixed powder is put into blender by funnel, blender is with the stirring rate of 600/min to mixing
Powder stirring is uniform, mixing time 14min；
D: compacting: the mixed powder after stirring is pressed into dry film, is then compressed on dry film by hot pressing complex method
The inside of Ti stick, and encapsulated holes are reserved at the center of Ti stick, the compound temperature range of hot pressing is 100 DEG C,；
E: addition: mixing merga pass blender for acrylamide and acrylic acid with 1: 1 ratio and stir evenly, acrylamide
The 50% of function core gross mass is accounted for acrylic acid, then mixed gel agent and methylene-bisacrylamide is mixed with 1: 2 ratio
Merga pass blender stirs evenly, and mixed gel agent and methylene-bisacrylamide account for the 38% of function core gross mass, so
The potassium chloride that concentration is 1~3M is added in blender afterwards to stir evenly, potassium chloride accounts for the 2% of the new gross mass of function, finally again
Tetrafluoro boric acid and hydrogen peroxide will be added with 1: 1 ratio in mixture, and is stirred evenly by blender, tetrafluoro boric acid and mistake
The ratio of hydrogen oxide accounts for the 10% of function core gross mass；
F: drying: mixing material is reacted into the concentration mixed and is stored by distilling box, is then placed in baking vessel
Oven on be dehydrated, baking time 45min, toasting indoor temperature is 150 DEG C, and mixing is reacted in concentration after baking
Material forms gelinite；
G: cooling: gelinite being taken out out of baking vessel, the gelinite of high-temperature process is stood, the temperature of high temperature gel body is made
Degree is down to room temperature；
H: filling: in the interior welds copper conductor of the encapsulated holes of Ti stick, while in the uniform gel filled body in the outside of Ti stick,
Gelinite is wrapped up by PVC shell, after gelinite filling, PVC shell is screwed into fastening；
I: encapsulation saves: the quality in order to guarantee the function core, after PVC shell screws fastening, by medical sponge to function
Energy core is wrapped up and is placed in vacuum box, is opened vacuum box when need to use and is needed immediately to make function core
With.
As a kind of optional technical solution of the invention: in step B, temperature range is 60 before active material powder mixes
DEG C, temperature range is 70 DEG C before conductive agent powder mixes, and temperature range is 70 DEG C before binder powder mixes.
As a kind of optional technical solution of the invention: in step E, first mixing acrylamide and acrylic acid in proportion
It closes, is stirred by blender with the rate of 750r/min, mixing time 10, then by mixed gel agent and methylene
Bisacrylamide is mixed with material is mixed, and is stirred evenly by blender with the rate of 750r/min, mixing time is
8min, then potassium chloride is mixed with material is mixed, it is stirred evenly by blender with the rate of 700r/min, mixing time
For 3min, finally tetrafluoro boric acid and hydrogen peroxide are mixed with material is mixed, by blender with the rate of 800r/min
It stirs evenly, mixing time 4min.
As a kind of optional technical solution of the invention: in step F, toasting indoor temperature with the speed liter of 10 DEG C/min
Temperature.
Function core can be made by above three groups of embodiments, wherein the mass effect of second group of embodiment production and processing
Preferably, it is mixed by active material powder, conductive agent powder and binder powder, then repressed equipment suppresses mixed powder
In the inside of Ti stick, electric current is conducted by copper conductor and mixed powder, the inner core of motor is made by mixed powder and Ti stick,
Then concentration reaction mixing material is formed into gelinite by oven dewatered drying, then gelinite is uniformly wrapped in Ti stick
Outer surface, then gelinite is fixed by PVC shell, keeps the total quality of the function core higher, when use is more steady
It is fixed.
It should be noted that in the present invention unless specifically defined or limited otherwise, fisrt feature is in second feature
It can be that the first and second features directly contact or the first and second features are by intermediary mediate contact "up" or "down".
Moreover, fisrt feature can be above the second feature " above ", " above " and " above " fisrt feature right above second feature or tiltedly
Top, or first feature horizontal height is merely representative of higher than second feature.Fisrt feature second feature " under ", " lower section " and
" following " can be fisrt feature and be directly under or diagonally below the second feature, or be merely representative of first feature horizontal height less than
Two features.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features,
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (10)
1. a kind of all-solid-state reference electrode Preparation equipment based on EB-PVD and SOL-GEL characterized by comprising
Agitating device (1) and solidification room (2), the upper surface of the agitating device (1) is fixedly connected with feed inlet (3), described to stir
The inside for mixing device (1) offers feeding-passage (4), and the feeding-passage (4) is located at the lower section of feed inlet (3), the charging
Mouth (3) and feeding-passage (4) are interconnected；
The bottom of the feeding-passage (4) offers stirred tank (5), and the inside of the agitating device (1) is far from feeding-passage (4)
Side offer the first rotation slot (6), the internal activity of first rotation slot (6) is connected with first gear (7), described
The side of one rotation slot (6) offers the second rotation slot (8), and the internal activity of second rotation slot (8) is connected with the second tooth
It takes turns (9), a middle side part of the second gear (9) is fixedly connected with shaft (10), and the shaft (10) is far from second gear (9)
One end sequentially pass through the side of the second rotation slot (8) and the side of agitating device (1) and be located at agitating device (1) outside；
It is fixedly connected with connecting shaft (11) in the middle part of the lower surface of the first gear (7), the connecting shaft (11) is far from the first tooth
Take turns the upper surface middle part of the one end through stirred tank (5) of (7) and the inside positioned at stirred tank (5), the bottom of the connecting shaft (11)
Multiple paddles (12) are fixedly connected in portion's circumferential direction；
It is offered transmission channel (13) in the middle part of the lower surface of the stirred tank (5), the internal activity peace of the transmission channel (13)
It equipped with connecting rod (14), is fixedly connected with sprue (15) at the top of the connecting rod (14), the side of the transmission channel (13)
It offers control flume (17), the bottom side of the connecting rod (14) is fixedly connected with control-rod (16), the control-rod (16)
Side of the one end far from connecting rod (14) through control flume (17) and the inside positioned at control flume (17)；
The inside of the control flume (17) is fixedly installed with articulation piece (19), the middle part and articulation piece (19) of the control-rod (16)
It is flexibly connected, the control-rod (16) is movably arranged on the inside of control flume (17), the control-rod by articulation piece (19)
(16) upper surface is fixedly connected with spring (18) far from the side of connecting rod (14), and the spring (18) is far from control-rod (16)
One end be fixedly connected on the upper surface side of control flume (17)；
The lower surface of the agitating device (1) is fixedly connected with connecting tube (20), and the bottom of the connecting tube (20) is fixedly connected
Have solidification room (2), the transmission channel (13) and connecting tube (20) are interconnected；
The one end of the connecting tube (20) far from agitating device (1) is through the upper surface middle part for solidifying room (2) and is fixedly connected with
One end of isocon (21), the connecting tube (20) is fixedly connected with the upper surface middle part of isocon (21), the isocon
(21) lower surface is fixedly connected with multiple branch pipes (22), is fixedly installed with support plate (23), institute in the middle part of the solidification room (2)
The upper surface for stating support plate (23) is fixedly installed with multiple coagulating basins (24), fixed peace in the middle part of the lower surface of solidification room (2)
Equipped with drying oven (25).
2. a kind of all-solid-state reference electrode Preparation equipment based on EB-PVD and SOL-GEL according to claim 1, special
Sign is:
The stirred tank (5) is in bucket type structure, is adapted in the middle part of the sprue (15) and the lower surface of stirred tank (5), described stifled
Inside of the top of block (15) in the middle part of the lower surface of stirred tank (5) and positioned at stirred tank (5).
3. a kind of all-solid-state reference electrode Preparation equipment based on EB-PVD and SOL-GEL according to claim 1, special
Sign is:
The quantity of the paddle (12) is no less than three, two neighboring paddle (12) spaced set, the paddle
(12) opening is offered in the middle part of.
4. a kind of all-solid-state reference electrode Preparation equipment based on EB-PVD and SOL-GEL according to claim 1, special
Sign is:
The shaft (10) runs through the top side of agitating device (1), shaft (10) position far from the one end of second gear (9)
Servo motor is connected in the one end of agitating device (1) outside.
5. a kind of all-solid-state reference electrode Preparation equipment based on EB-PVD and SOL-GEL according to claim 1, special
Sign is:
First rotation slot (6) is mutually perpendicular to the second rotation slot (8), first rotation slot (6) and the second rotation slot (8)
It being interconnected, the first gear (7) is bevel gear, the one of the upper surface side of the first gear (7) and second gear (9)
Side engagement connection.
6. a kind of all-solid-state reference electrode Preparation equipment based on EB-PVD and SOL-GEL according to claim 1, special
Sign is:
The branch pipe (22) is distributed parallelly on the lower surface of isocon (21), and the distance between two neighboring branch pipe (22) is equal；
The upper surface of solidification room (2) offers multiple drying holes (26), and the drying hole (26) is to solidify the centers of room (2)
Point is that center of circle circular array is distributed.
7. a kind of method of the all-solid-state reference electrode preparation based on EB-PVD and SOL-GEL, which is characterized in that including following step
It is rapid:
A: deposition: by EP-PVD technology, deposition obtains bianry alloy film from Ti stick matrix, and the bianry alloy of acquirement is thin
The Ti stick of film, which is placed in high temperature furnace, carries out oxidation processes, and oxidizing temperature is 600 DEG C~800 DEG C, and oxidization time is 8~10min,
Heating rate in high temperature furnace is 10 DEG C~15 DEG C/min；
B: mixing: by active material powder, conductive agent powder, binder powder according to 30~100: 2~10: 5~15 ratio
It is stirred；
C: stirring: mixed powder is put into blender by funnel, and blender is with the stirring rate of 500~800/min to mixed
It is uniform to close powder stirring, mixing time is 10~20min；
D: compacting: the mixed powder after stirring is pressed into dry film, dry film is then compressed on by Ti stick by hot pressing complex method
Inside, and the center of Ti stick reserve encapsulated holes, the compound temperature range of hot pressing be 80 DEG C~130 DEG C,；
E: addition: mixing merga pass blender for acrylamide and acrylic acid with 1: 1 ratio and stir evenly, acrylamide and third
Olefin(e) acid accounts for the 40%~60% of function core gross mass, then by mixed gel agent and methylene-bisacrylamide with 1: 2 ratio
Mixed merga pass blender stirs evenly, mixed gel agent and methylene-bisacrylamide account for function core gross mass 30%~
50%, the potassium chloride that concentration is 1~3M is then added in blender and stirs evenly, potassium chloride accounts for the 2% of the new gross mass of function,
Finally tetrafluoro boric acid and hydrogen peroxide will be added again with 1: 1 ratio in mixture, and is stirred evenly by blender, tetrafluoro boron
The ratio of acid and hydrogen peroxide accounts for the 10% of function core gross mass；
F: drying: reacting mixing material for the concentration mixed and stored by distilling box, is then placed on the indoor baking of baking
It is dehydrated on oven, baking time is 30~50min, and toasting indoor temperature is 140~170 DEG C, and the concentration after baking is anti-
Mixing material is answered to form gelinite；
G: cooling: gelinite being taken out out of baking vessel, the gelinite of high-temperature process is stood, the temperature of high temperature gel body is dropped
To room temperature；
H: filling: in the interior welds copper conductor of the encapsulated holes of Ti stick, while in the uniform gel filled body in the outside of Ti stick, pass through
PVC shell wraps up gelinite, and after gelinite filling, PVC shell is screwed fastening；
I: encapsulation saves: the quality in order to guarantee the function core, after PVC shell screws fastening, by medical sponge to function core
Wrapped up and be placed in vacuum box, when need to use open vacuum box and need immediately to function core carry out using.
8. a kind of method of all-solid-state reference electrode preparation based on EB-PVD and SOL-GEL according to claim 7,
It is characterized in that:
In the step B, temperature range is 50~70 DEG C before active material powder mixes, temperature range before conductive agent powder mixes
It is 60 DEG C~80 DEG C, temperature range is 80 DEG C~100 DEG C before binder powder mixes.
9. a kind of method of all-solid-state reference electrode preparation based on EB-PVD and SOL-GEL according to claim 7,
It is characterized in that:
In the step E, acrylamide and acrylic acid are mixed in proportion first, by blender with 700~800r/min's
Rate is stirred, and mixing time is 6~10min, then stirs mixed gel agent and methylene-bisacrylamide with mixing
Material mixing is mixed, is stirred evenly by blender with the rate of 700~800r/min, mixing time is 8~15min, then by chlorine
Change potassium and mixed with material is mixed, stirred evenly by blender with the rate of 700~800r/min, mixing time for 3~
5min finally mixes tetrafluoro boric acid and hydrogen peroxide with material is mixed, by blender with the speed of 700~800r/min
Rate stirs evenly, and mixing time is 4~7min.
10. a kind of method of all-solid-state reference electrode preparation based on EB-PVD and SOL-GEL according to claim 7,
It is characterized by:
In the step F, toasts indoor temperature and heated up with the speed of 10 DEG C/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112011758A (en) * | 2020-07-16 | 2020-12-01 | 西安怡速安智能科技有限公司 | Anode production process for improving anode activity by electrochemical electrode PVD method |
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| CN102087241A (en) * | 2010-11-17 | 2011-06-08 | 哈尔滨工业大学 | Method for preparing all-solid-state reference electrode (RE) based on EB-PVD (electron beam physical vapor deposition) and Sol-Gel |
| CN103045884A (en) * | 2013-01-24 | 2013-04-17 | 哈尔滨工业大学 | Device and method for preparing large-size light alloy semi-solid billet |
| CN204973099U (en) * | 2015-08-11 | 2016-01-20 | 东北石油大学 | Evaporator with cooling device |
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| CN102087241A (en) * | 2010-11-17 | 2011-06-08 | 哈尔滨工业大学 | Method for preparing all-solid-state reference electrode (RE) based on EB-PVD (electron beam physical vapor deposition) and Sol-Gel |
| CN103045884A (en) * | 2013-01-24 | 2013-04-17 | 哈尔滨工业大学 | Device and method for preparing large-size light alloy semi-solid billet |
| CN204973099U (en) * | 2015-08-11 | 2016-01-20 | 东北石油大学 | Evaporator with cooling device |
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