CN106083053B - A kind of preparation method of marmatite electrode - Google Patents
A kind of preparation method of marmatite electrode Download PDFInfo
- Publication number
- CN106083053B CN106083053B CN201610464242.5A CN201610464242A CN106083053B CN 106083053 B CN106083053 B CN 106083053B CN 201610464242 A CN201610464242 A CN 201610464242A CN 106083053 B CN106083053 B CN 106083053B
- Authority
- CN
- China
- Prior art keywords
- marmatite
- cylinder
- sodium chloride
- powder
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/547—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on sulfides or selenides or tellurides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Immunology (AREA)
- Inorganic Chemistry (AREA)
- Pathology (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biodiversity & Conservation Biology (AREA)
- Ecology (AREA)
- Environmental & Geological Engineering (AREA)
- Environmental Sciences (AREA)
- Powder Metallurgy (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of preparation methods of marmatite electrode, it includes selecting marmatite particle；It will be dried for standby after the marmatite particle cleaning selected；Marmatite 0.8 ~ 1.0g of particle after drying is weighed, is ground into the powder of 200 mesh or more, 1MPa conditions are wrapped up after depressing to marmatite cylinder with silver foil in powder compressing machine；The powder that sodium chloride is ground into 200 mesh or more is placed in baking oven at a temperature of 150 DEG C and dries 2 hours；The sodium chloride cylindrical samples for including marmatite cylinder are prepared with the sodium chloride powder after drying；The sodium chloride cylindrical samples for including marmatite cylinder are put into high pressure assembling block, temperature-pressure sintering is carried out；Sample sanding and polishing after the completion of sintering is up to marmatite electrode；It is crisp that the present invention solves prior art marmatite, and poor ductility and marmatite and other sulfide mineral symbiosis influence the factors such as marmatite electrochemical corrosion result, and existing marmatite electrode is difficult that processing such as prepares at the technical problems.
Description
Technical field
The invention belongs to marmatite electrode fabrication more particularly to a kind of preparation methods of marmatite electrode.
Background technology
Zincblende is present in hydrothermal deposit as most wide zinc mineral is distributed, is the important mineral products of extracting zinc.Naturally deposit
The general iron content of zincblende, referred to as marmatite, wherein iron-holder reach as high as 30%.Increase with iron content, marmatite
It darkens, pale yellow, brown even black is presented.The electrochemical corrosion behavior that marmatite is studied in hydrothermal system, helps
In the generation, composition and the change procedure that understand hydrothermal deposit, theoretical foundation is provided for ore-dressing technique.
Natural marmatite often with galena sulfides mineral intergrowth.Primary battery chemical action between paragenous mineral
Galena electrochemical corrosion course can be interfered, influence its essential nature.Therefore, preparing pure marmatite electrode becomes
The necessary condition of electrochemical corrosion research.However, it is extremely difficult to the very high natural block marmatite of purity is found as research object.
In addition, natural marmatite poor crystal form, poor ductility, it is difficult to be processed into the required electrode of electrochemical research.
Invention content
The technical problem to be solved in the present invention：A kind of preparation method of marmatite electrode is provided, to solve the prior art
Marmatite is crisp, poor ductility and marmatite and other sulfide mineral symbiosis, and the primary battery between paragenous mineral is made
With that can influence the factors such as marmatite electrochemical corrosion result, existing marmatite electrode is difficult that the technologies such as processing preparation are asked
Topic.
Technical solution of the present invention：
A kind of preparation method of marmatite electrode, it includes
Step 1 selects marmatite particle；
Step 2 will be dried for standby after the marmatite particle cleaning selected；
Step 3 weighs marmatite 0.8 ~ 1.0g of particle after drying, the powder of 200 mesh or more is ground into, in powder pressure
1MPa conditions are wrapped up after depressing to marmatite cylinder with silver foil in piece machine；
Step 4 after sodium chloride is ground into the powder of 200 mesh or more, is placed in baking oven at a temperature of 150 DEG C and dries 2 hours；
Step 5 prepares the sodium chloride cylindrical samples for including marmatite cylinder with the sodium chloride powder after drying；
The sodium chloride cylindrical samples for including marmatite cylinder are put into high pressure assembling block by step 6, are heated
Pressure sintering；
Sample sanding and polishing after the completion of step 7, sintering is up to marmatite electrode.
The method that step 1 selects marmatite particle is：Rock containing marmatite is broken into 80-100 mesh, in binocular
The marmatite that purity is 95% or more is picked out under mirror.
Furnace drying method is after marmatite particle cleaning described in step 2：It is cleaned by ultrasonic 10-20min with acetone, then with anhydrous
Ethyl alcohol cleans, and is subsequently placed in baking oven 5-30min at a temperature of 30-60 DEG C.
The method of sodium chloride cylinder for including marmatite cylinder is prepared described in step 5 is：Sodium chloride powder is existed
It is pressed into cylinder in powder compressing machine, the marmatite cylinder wrapped up with silver foil is then placed on sodium chloride cylinder upper surface
Centre position, add sodium chloride powder covering, be compacted under the conditions of 1MPa in powder compressing machine, obtain including marmatite
The sodium chloride cylinder of cylinder completes preparation of samples.
Sample described in step 6 is put into high pressure assembling block, and its implementation includes：
Step 6.1 chooses one piece of pyrophyllite block, and a circular through hole is made at pyrophyllite block center；
Step 6.2, in one circular graphite heater furnace of circular through hole inner sleeve；
The sodium chloride cylindrical samples for including marmatite cylinder are placed among step 6.3, graphite heater furnace；
Step 6.4 seals circular graphitic heating furnace upper and lower ends pyrophillite plug.
Temperature-pressure sintering described in step 6 is that high pressure assembling block is put into temperature-pressure in 6*600t cubic hinge press to burn
Knot sets pressure as 0.2-2.0 GPa, and set temperature is 200-700 DEG C, reaction time 10-90min.
It is provided with thermocouple in the high pressure assembling block.
Described in step 7 by the sample sanding and polishing after the completion of sintering, method is：
Marmatite cylinder after the completion of sintering is sticked to AB glue in stud by step 7.1；
Marmatite cylinder after the completion of sintering is processed into round platform by step 7.2 with grinding machine；
Step 7.3, the big small end face sanding and polishing by round platform；
Round platform after polishing is cleaned by ultrasonic 10-20min by step 7.4 in acetone, is put into inert gas after natural drying
It is saved backup in atmosphere or vacuum environment.
Beneficial effects of the present invention：
The present invention, using the marmatite selected as raw material, is stabilized under conditions of high temperature and pressure in marmatite
Within the scope of pressure and temperature, the recrystallization method reacted by solid-state diffusion eliminates the interface between crystal grain, allows crystal grain
It grows up, so that marmatite powder is formed bulk, reach required hardness and strength, and be processed into shape, successfully prepare phase
The marmatite electrode purer than naturally；It is crisp to solve prior art marmatite, poor ductility and marmatite and its
His sulfide mineral symbiosis, and the Galvanic interaction between paragenous mineral can influence the factors such as marmatite electrochemical corrosion result,
Existing marmatite electrode is difficult the technical problems such as processing preparation.
Specific implementation mode：
A kind of preparation method of marmatite electrode, it includes
Step 1 selects marmatite particle；
Step 2 will be dried for standby after the marmatite particle cleaning selected；
Step 3 weighs marmatite 0.8 ~ 1.0g of particle after drying, the powder of 200 mesh or more is ground into, in powder pressure
1MPa conditions are wrapped up after depressing to marmatite cylinder with silver foil in piece machine；
Step 4 after sodium chloride is ground into the powder of 200 mesh or more, is placed in baking oven at a temperature of 150 DEG C and dries 2 hours；
Step 5 prepares the sodium chloride cylindrical samples for including marmatite cylinder with the sodium chloride powder after drying；
The sodium chloride cylindrical samples for including marmatite cylinder are put into high pressure assembling block by step 6, are heated
Pressure sintering；
Sample sanding and polishing after the completion of step 7, sintering is up to marmatite electrode.
The method that step 1 selects marmatite particle is：Rock containing marmatite is broken into 80-100 mesh, in binocular
The marmatite that purity is 95% or more is picked out under mirror.
Furnace drying method is after marmatite particle cleaning described in step 2：It is cleaned by ultrasonic 10-20min with acetone, then with anhydrous
Ethyl alcohol cleans, and is subsequently placed in baking oven 5-30min at a temperature of 30-60 DEG C.
The method of sodium chloride cylinder for including marmatite cylinder is prepared described in step 5 is：Sodium chloride powder is existed
It is pressed into cylinder in powder compressing machine, the marmatite cylinder wrapped up with silver foil is then placed on sodium chloride cylinder upper surface
Centre position, add sodium chloride powder covering, be compacted under the conditions of 1MPa in powder compressing machine, obtain including marmatite
The sodium chloride cylinder of cylinder completes preparation of samples.
Sample described in step 6 is put into high pressure assembling block, and its implementation includes：
Step 6.1 chooses one piece of pyrophyllite block, and a circular through hole is made at pyrophyllite block center；
Step 6.2, in one circular graphite heater furnace of circular through hole inner sleeve；
The sodium chloride cylindrical samples for including marmatite cylinder are placed among step 6.3, graphite heater furnace；
Step 6.4 seals circular graphitic heating furnace upper and lower ends pyrophillite plug.
Temperature-pressure sintering described in step 6 is that high pressure assembling block is put into temperature-pressure in 6*600t cubic hinge press to burn
Knot sets pressure as 0.2-2.0 GPa, and set temperature is 200-700 DEG C, reaction time 10-90min.
It is provided with thermocouple in the high pressure assembling block.
Described in step 7 by the sample sanding and polishing after the completion of sintering, method is：
Marmatite cylinder after the completion of sintering is sticked to AB glue in stud by step 7.1；
Marmatite cylinder after the completion of sintering is processed into round platform by step 7.2 with grinding machine；
Step 7.3, the big small end face sanding and polishing by round platform；
Round platform after polishing is cleaned by ultrasonic 10-20min by step 7.4 in acetone, is put into inert gas after natural drying
It is saved backup in atmosphere or vacuum environment.
Case study on implementation 1：
Rock containing marmatite is broken into 80-100 mesh, iron of the purity more than 95% is picked out under binocular and dodges zinc
Mine particle is cleaned by ultrasonic 10-20min with acetone, then clean with washes of absolute alcohol, is subsequently placed in 30-60 DEG C of temperature in baking oven
It is dried for standby after lower 5-30min.1.0g marmatite particles are weighed, the powder of 200 mesh or more are ground into, in pressed powder
1MPa conditions depress to cylinder in machine, are wrapped up with silver foil.The powder that sodium chloride is also ground into 200 mesh or more is weighed, is set
Drying is spare as transmission medium after 2h at a temperature of 150 DEG C in baking oven.0.67g sodium chloride is weighed, is pressed in powder compressing machine
At cylindric, then marmatite cylinder is placed on to the centre position of sodium chloride cylinder upper surface, then pour into 0.75g chlorinations
Sodium covers, and is compacted under the conditions of 1MPa in pressed powder, obtains the sodium chloride cylinder for including marmatite cylinder, completes sample
Product prepare.High pressure assembles block assembling mode：
The through-hole of a diameter of 14mm is beaten at the pyrophyllite block center of 32 × 32mm；
It is 14mm that an outer diameter is covered inside pyrophyllite block hole, and internal diameter is the graphite heater furnace of 10mm；
The sodium chloride cylinder for including marmatite cylinder is put among graphite heater furnace, is up and down a diameter of 10mm
Pyrophillite plug.
So far, high pressure assembling block is completed, and the size that mesohigh assembling block is related to can be according to the ruler of marmatite electrode
It is very little specifically to determine；In the assembling block, pyrophillite and sodium chloride make transmission medium, and graphite furnace makees heating furnace, and thermocouple makees temperature control
Device.The advantages of high pressure of the present invention assembling block is：The temperature fed back by thermocouple using thermocouple temperature control, heating system
Heating power is adjusted, to change temperature, the immediately monitoring to temperature may be implemented in this method, is suitable for temperature measurement accuracy
It is required that high experiment；Pyrophillite has good pressure transmission, machining property, heat insulation as level-one transmission medium
Property and insulating properties, sodium chloride are a kind of low sheraing materials, as two level transmission medium, keep the pressure in cavity relatively uniform, and
Its good airproof performance；For graphite furnace as heating furnace, temperature uniformity is high.After the completion of high pressure assembles block, domestic 6* is put it into
Temperature-pressure is sintered in 600t cubic hinge press, sets pressure as 2 GPa, and set temperature is 700 DEG C, reaction time 90min,
After the completion of reaction, sample is taken out, purity is obtained and is more than 95%, density is the marmatite cylinder of 3.8-4.5.It is of the invention high
The advantages of warm High-Voltage Experimentation condition setting is：The temperature, pressure condition of setting is the condition that marmatite is stablized, at this
Under part, marmatite will not be changed into other substances；The temperature, pressure condition of selection is conducive to marmatite recrystallization, energy
Access the wanted hardness of electrode.Pure iron zincblende cylinder is sticked to AB glue in stud, with grinding machine by above-mentioned thermal sintering
Cylinder is processed into round platform, and by the big small end face sanding and polishing of round platform.Round platform after polishing is cleaned by ultrasonic 10- in acetone
20min is put into atmosphere of inert gases or vacuum environment and saves backup after natural drying.
Case study on implementation 2：
Rock containing marmatite is broken into 80-100 mesh, iron of the purity more than 95% is picked out under binocular and dodges zinc
Mine particle is cleaned by ultrasonic 10-20min with acetone, then clean with washes of absolute alcohol, is subsequently placed in 30-60 DEG C of temperature in baking oven
It is dried for standby after lower 5-30min.1.0g marmatite particles are weighed, the powder of 200 mesh or more are ground into, in pressed powder
1MPa conditions depress to cylinder in machine, are wrapped up with silver foil.The powder that sodium chloride is also ground into 200 mesh or more is weighed, is set
Drying is spare as transmission medium after 2h at a temperature of 150 DEG C in baking oven.0.67g sodium chloride is weighed, is pressed in powder compressing machine
At cylindric, then marmatite cylinder is placed on to the centre position of sodium chloride cylinder upper surface, then pour into 0.75g chlorinations
Sodium covers, and is compacted under the conditions of 1MPa in pressed powder, obtains the sodium chloride cylinder for including marmatite cylinder, completes sample
Product prepare.High pressure assembles block assembling mode：
The through-hole of a diameter of 14mm is beaten at the pyrophyllite block center of 32 × 32mm；
It is 14mm that an outer diameter is covered inside pyrophyllite block hole, and internal diameter is the graphite heater furnace of 10mm；
The sodium chloride cylinder for including marmatite cylinder is put among graphite heater furnace, is up and down a diameter of 10mm
Pyrophillite plug.
So far, high pressure assembling block is completed, and the size that mesohigh assembling block is related to can be according to the ruler of marmatite electrode
It is very little specifically to determine；In the assembling block, pyrophillite and sodium chloride make transmission medium, and graphite furnace makees heating furnace, and thermocouple makees temperature control
Device.The advantages of high pressure of the present invention assembling block is：The temperature fed back by thermocouple using thermocouple temperature control, heating system
Heating power is adjusted, to change temperature, the immediately monitoring to temperature may be implemented in this method, is suitable for temperature measurement accuracy
It is required that high experiment；Pyrophillite has good pressure transmission, machining property, heat insulation as level-one transmission medium
Property and insulating properties, sodium chloride are a kind of low sheraing materials, as two level transmission medium, keep the pressure in cavity relatively uniform, and
Its good airproof performance；For graphite furnace as heating furnace, temperature uniformity is high.After the completion of high pressure assembles block, domestic 6* is put it into
Temperature-pressure is sintered in 600t cubic hinge press, sets pressure as 1 GPa, and set temperature is 500 DEG C, reaction time 60min,
After the completion of reaction, sample is taken out, purity is obtained and is more than 95%, density is the marmatite cylinder of 3.8-4.5.It is of the invention high
The advantages of warm High-Voltage Experimentation condition setting is：The temperature, pressure condition of setting is the condition that marmatite is stablized, at this
Under part, marmatite will not be changed into other substances；The temperature, pressure condition of selection is conducive to marmatite recrystallization, energy
Access the wanted hardness of electrode.Pure iron zincblende cylinder is sticked to AB glue in stud, with grinding machine by above-mentioned thermal sintering
Cylinder is processed into round platform, and by the big small end face sanding and polishing of round platform.Round platform after polishing is cleaned by ultrasonic 10- in acetone
20min is put into atmosphere of inert gases or vacuum environment and saves backup after natural drying.
Case study on implementation 3：
Rock containing marmatite is broken into 80-100 mesh, iron of the purity more than 95% is picked out under binocular and dodges zinc
Mine particle is cleaned by ultrasonic 10-20min with acetone, then clean with washes of absolute alcohol, is subsequently placed in 30-60 DEG C of temperature in baking oven
It is dried for standby after lower 5-30min.1.0g marmatite particles are weighed, the powder of 200 mesh or more are ground into, in pressed powder
1MPa conditions depress to cylinder in machine, are wrapped up with silver foil.The powder that sodium chloride is also ground into 200 mesh or more is weighed, is set
Drying is spare as transmission medium after 2h at a temperature of 150 DEG C in baking oven.0.67g sodium chloride is weighed, is pressed in powder compressing machine
At cylindric, then marmatite cylinder is placed on to the centre position of sodium chloride cylinder upper surface, then pour into 0.75g chlorinations
Sodium covers, and is compacted under the conditions of 1MPa in pressed powder, obtains the sodium chloride cylinder for including marmatite cylinder, completes sample
Product prepare.High pressure assembles block assembling mode：
The through-hole of a diameter of 14mm is beaten at the pyrophyllite block center of 32 × 32mm；
It is 14mm that an outer diameter is covered inside pyrophyllite block hole, and internal diameter is the graphite heater furnace of 10mm；
The sodium chloride cylinder for including marmatite cylinder is put among graphite heater furnace, is up and down a diameter of 10mm
Pyrophillite plug.
So far, high pressure assembling block is completed, and the size that mesohigh assembling block is related to can be according to the ruler of marmatite electrode
It is very little specifically to determine；In the assembling block, pyrophillite and sodium chloride make transmission medium, and graphite furnace makees heating furnace, and thermocouple makees temperature control
Device.The advantages of high pressure of the present invention assembling block is：The temperature fed back by thermocouple using thermocouple temperature control, heating system
Heating power is adjusted, to change temperature, the immediately monitoring to temperature may be implemented in this method, is suitable for temperature measurement accuracy
It is required that high experiment；Pyrophillite has good pressure transmission, machining property, heat insulation as level-one transmission medium
Property and insulating properties, sodium chloride are a kind of low sheraing materials, as two level transmission medium, keep the pressure in cavity relatively uniform, and
Its good airproof performance；For graphite furnace as heating furnace, temperature uniformity is high.After the completion of high pressure assembles block, domestic 6* is put it into
Temperature-pressure is sintered in 600t cubic hinge press, set pressure as 0.2 GPa, and set temperature is 200 DEG C, and the reaction time is
After the completion of reaction, sample is taken out by 10min, is obtained purity and is more than 95%, density is the marmatite cylinder of 3.8-4.5.This
Invention high temperature and pressure experiment condition set the advantages of be：The temperature, pressure condition of setting is the condition that marmatite is stablized,
With this condition, marmatite will not be changed into other substances；The temperature, pressure condition of selection is conducive to marmatite weight
Crystallization, can obtain the wanted hardness of electrode.Pure iron zincblende cylinder is sticked to AB glue in stud, with grinding machine by above-mentioned sintering
The cylinder of forming is processed into round platform, and by the big small end face sanding and polishing of round platform.Round platform after polishing is ultrasonic in acetone
10-20min is cleaned, is put into atmosphere of inert gases or vacuum environment and saves backup after natural drying.
Claims (7)
1. a kind of preparation method of marmatite electrode, it includes
Step 1 selects marmatite particle；
Step 2 will be dried for standby after the marmatite particle cleaning selected；
Step 3 weighs marmatite 0.8 ~ 1.0g of particle after drying, grind into powder, the 1MPa conditions in powder compressing machine
It is wrapped up with silver foil after depressing to marmatite cylinder；
Step 4 after sodium chloride is ground into the powder of 200 mesh or more, is placed in baking oven at a temperature of 150 DEG C and dries 2 hours；
Step 5 prepares the sodium chloride cylindrical samples for including marmatite cylinder with the sodium chloride powder after drying；
The sodium chloride cylindrical samples for including marmatite cylinder are put into high pressure assembling block by step 6, carry out temperature-pressure
Sintering；Temperature-pressure sintering described in step 6 is that high pressure assembling block is put into temperature-pressure in 6*600t cubic hinge press to be sintered,
Pressure is set as 0.2-2.0 GPa, set temperature is 200-700 DEG C, reaction time 10-90min；
Sample sanding and polishing after the completion of step 7, sintering is up to marmatite electrode.
2. a kind of preparation method of marmatite electrode according to claim 1, it is characterised in that：Step 1 selects iron sudden strain of a muscle
The method of zinc ore particle is：Rock containing marmatite is broken into 80-100 mesh, picked out under binocular purity be 95% with
On marmatite.
3. a kind of preparation method of galena electrode according to claim 1, it is characterised in that：Iron described in step 2 dodges zinc
Furnace drying method is after mine particle cleaning：It is cleaned by ultrasonic 10-20min with acetone, then with washes of absolute alcohol, is subsequently placed in baking oven
5-30min at a temperature of 30-60 DEG C.
4. a kind of preparation method of marmatite electrode according to claim 1, it is characterised in that：It is prepared described in step 5
The method for including the sodium chloride cylinder of marmatite cylinder is：Sodium chloride powder is pressed into cylinder in powder compressing machine
Then the marmatite cylinder wrapped up with silver foil is placed on the centre position of sodium chloride cylinder upper surface, adds chlorine by body
Change the covering of sodium powder end, is compacted under the conditions of 1MPa in powder compressing machine, obtains the sodium chloride cylinder for including marmatite cylinder
Body completes preparation of samples.
5. a kind of preparation method of marmatite electrode according to claim 1, it is characterised in that：Sample described in step 6
It is put into high pressure assembling block, its implementation includes：
Step 6.1 chooses one piece of pyrophyllite block, and a circular through hole is made at pyrophyllite block center；
Step 6.2, in one circular graphite heater furnace of circular through hole inner sleeve；
The sodium chloride cylindrical samples for including marmatite cylinder are placed among step 6.3, graphite heater furnace；
Step 6.4 seals circular graphitic heating furnace upper and lower ends pyrophillite plug.
6. a kind of preparation method of marmatite electrode according to claim 5, it is characterised in that：The high pressure assembles block
Inside it is provided with thermocouple.
7. a kind of preparation method of marmatite electrode according to claim 1, it is characterised in that：General described in step 7
Sample sanding and polishing after the completion of sintering, method are：
Marmatite cylinder after the completion of sintering is sticked to AB glue in stud by step 7.1；
Marmatite cylinder after the completion of sintering is processed into round platform by step 7.2 with grinding machine；
Step 7.3, the big small end face sanding and polishing by round platform；
Round platform after polishing is cleaned by ultrasonic 10-20min by step 7.4 in acetone, is put into atmosphere of inert gases after natural drying
Or it is saved backup in vacuum environment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610464242.5A CN106083053B (en) | 2016-06-24 | 2016-06-24 | A kind of preparation method of marmatite electrode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610464242.5A CN106083053B (en) | 2016-06-24 | 2016-06-24 | A kind of preparation method of marmatite electrode |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106083053A CN106083053A (en) | 2016-11-09 |
| CN106083053B true CN106083053B (en) | 2018-10-19 |
Family
ID=57252373
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610464242.5A Expired - Fee Related CN106083053B (en) | 2016-06-24 | 2016-06-24 | A kind of preparation method of marmatite electrode |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106083053B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101307489A (en) * | 2008-02-02 | 2008-11-19 | 中国科学院物理研究所 | Halogen-containing high temperature superconductor crystal and method for making same |
| CN103439384A (en) * | 2013-08-26 | 2013-12-11 | 中国科学院地球化学研究所 | Mineral working electrode for electrochemical test of high-pressure hydrothermal system and preparation method of mineral working electrode |
| CN203396743U (en) * | 2013-08-26 | 2014-01-15 | 中国科学院地球化学研究所 | Mineral work electrode for electrochemical test of high-pressure hydrothermal system |
| CN104659034A (en) * | 2015-02-10 | 2015-05-27 | 中国科学院物理研究所 | Ferroelectric unit based on LaMn3Cr4O12 and ferroelectric memory |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7128547B2 (en) * | 2004-01-13 | 2006-10-31 | Chien-Min Sung | High pressure split die and associated methods |
-
2016
- 2016-06-24 CN CN201610464242.5A patent/CN106083053B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101307489A (en) * | 2008-02-02 | 2008-11-19 | 中国科学院物理研究所 | Halogen-containing high temperature superconductor crystal and method for making same |
| CN103439384A (en) * | 2013-08-26 | 2013-12-11 | 中国科学院地球化学研究所 | Mineral working electrode for electrochemical test of high-pressure hydrothermal system and preparation method of mineral working electrode |
| CN203396743U (en) * | 2013-08-26 | 2014-01-15 | 中国科学院地球化学研究所 | Mineral work electrode for electrochemical test of high-pressure hydrothermal system |
| CN104659034A (en) * | 2015-02-10 | 2015-05-27 | 中国科学院物理研究所 | Ferroelectric unit based on LaMn3Cr4O12 and ferroelectric memory |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106083053A (en) | 2016-11-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105973796B (en) | A kind of preparation method of chalcopyrite electrode | |
| CN106044867B (en) | A kind of preparation method of pyrite electrode | |
| CN106205857B (en) | A kind of preparation method of magnetic iron ore electrode | |
| CN106082350B (en) | A kind of method for preparing siderite at high temperature under high pressure | |
| CN101891214B (en) | Preparation method for synthesizing boron carbide powder at low temperature | |
| CN114702316B (en) | Preparation method and application of low-cost high-purity graphite material | |
| CN106744915A (en) | A kind of cellulose base graphitized material and preparation method thereof | |
| CN102268686A (en) | Electrochemical method for reducing solid metal oxide in molten salt to synthesize high-melting-point metal carbide under low temperature | |
| CN106092687B (en) | A kind of preparation method of galena electrode | |
| CN106830971A (en) | A kind of preparation method of MAX phases porous ceramics | |
| KR101137119B1 (en) | Method of producing magnesium-based hydrides | |
| CN108074751A (en) | A kind of flexible 3 D porous carbon materials and its preparation method and application | |
| CN106025235B (en) | A kind of preparation method of lithium ion battery graphene/SiC composite negative pole materials | |
| CN106892417A (en) | A kind of preparation method and application of konjaku flour base porous carbon material | |
| CN102897753B (en) | Preparation method for graphite with high thermal conductivity | |
| CN106083053B (en) | A kind of preparation method of marmatite electrode | |
| CN1978099A (en) | PbTe powde material formation preparing method | |
| CN112299482B (en) | Method for reducing thermal conductivity of bismuth sulfide thermoelectric material | |
| CN117393758A (en) | Hard carbon negative electrode material for sodium electricity and preparation method and application thereof | |
| CN110256079A (en) | A kind of preparation method of high-purity compact mispickel electrode | |
| CN101748304A (en) | Method and special sintering furnace for producing hard alloy | |
| CN107634183A (en) | The method that sulphur galvanic anode is prepared using protein | |
| CN106384826B (en) | Carbon coating vanadium-lithium phosphate powder for lithium preparation method for lithium ion cell electrode | |
| CN104477979A (en) | Method for preparing LiTi204 powder material | |
| CN109761609A (en) | A kind of manufacturing process and its process units of high-heat resistance shock resistant graphite electrode |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20181019 Termination date: 20210624 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |