CN109956750A - The preparation method of Alkali metal thermoelectric converter porous silicon carbide titanium electrode material - Google Patents
The preparation method of Alkali metal thermoelectric converter porous silicon carbide titanium electrode material Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/5607—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 carbides or oxycarbides based on refractory metal carbides
- C04B35/5611—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 carbides or oxycarbides based on refractory metal carbides based on titanium carbides
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Abstract
The invention discloses a kind of preparation method of Alkali metal thermoelectric converter porous silicon carbide titanium electrode material, the technical issues of the practicability is poor for solving existing porous silicon carbide titanium electrode material preparation method.Technical solution is that butyl titanate is dissolved in dehydrated alcohol, and stirring is added dropwise acetic acid, is made for solution A.Nitre acid for adjusting pH is used after dehydrated alcohol is mixed with deionized water, and B solution is made.B liquid is added dropwise in A liquid, with nitric acid regulation system pH value, aqueous sucrose solution is added dropwise and obtains the colloidal sol of titanium carbide, becomes stable gel after ageing.Gel is dried, is ground, compression moulding, calcines and is cooled to room temperature.After being surface-treated to BASE pipe, using silk screen print method, titanium carbide active electrode material is assembled on surface treated BASE tube cathode and anode, obtains porous silicon carbide Ti electrode finally by heating BASE pipe.The present invention realizes safely preparing for porous silicon carbide titanium electrode material.
Description
Technical field
The present invention relates to a kind of porous silicon carbide titanium electrode material preparation method, in particular to a kind of Alkali metal thermoelectric converter
The preparation method of porous silicon carbide titanium electrode material.
Background technique
Alkali metal thermoelectric converter abbreviation AMTEC is using β " alumina solid electrolyte as ion-permselective film, with
Liquid alkali metal or gaseous alkali metal are the direct switching device of thermoelectric energy of working medium.Be applicable in heat source temperature range be 900~
1300K.Theoretically, conversion efficiency of thermoelectric is up to 30%~40%.AMTEC is suitable for a variety of shapes such as nuclear energy, fossil energy, solar energy
The heat source of formula is that a kind of structure is simple, reliable operation, the thermoelectric energy conversion equipment for having higher power density, high effect cleaning.No
By in ground or space, there is good application prospect.
In alkali metal thermo-electric conversion equipment, electrode material used is very big on the influence of its heat to electricity conversion performance, and very
Decide the length in its service life in big degree.The electrode material of AMTEC is mainly include the following types: Mo, transition metal carbide
NbC、Ta2C and titanium carbide, transition metal nitride NbN, ZrN and TiN, transition metal boride TiB2And alloy electrode WPt2
And WRh3.Titanium carbide porous film electrode has porosity characteristic and good electric conductivity, on the one hand allows the sodium ion ionized
Through electrode gap, on the other hand it is also conducting element, will be loaded outside conduct current, while the electrode material is in AMTEC work
It does not undergo phase transition, will not be corroded at a temperature of work by alkali metal working medium.
" Tsuchida K, Nagata T, Nakata H, the et al.LaB6and TiB2electrodes for of document 1
the alkali metal thermoelectric converter[J].Journal of Materials Science,
1998,33 (3): 755-762 " discloses a kind of preparation method of Alkali metal thermoelectric converter porous silicon carbide titanium electrode material, should
Method is to mix TiC powder with organic carrier terpinol and ethyl cellulose, obtains the lotion that powder content is 20%, will
Lotion is dried 20 minutes in air at 150 DEG C, and in Ar-H at 900 or 1000 DEG C2Atmosphere or NH3-H2It is fired in atmosphere
1 or 3 hour, gained lotion is sprayed on beta oxidation aluminum pipe finally by sieve.But the preparation method needs to use hydrogen, system
It is standby that safety is lower, preparation method is complicated, preparation cost is higher, is difficult to realize the preparation of high-volume coating material.
Summary of the invention
In order to overcome the shortcomings of existing porous silicon carbide titanium electrode material preparation method, the practicability is poor, and the present invention provides a kind of alkali
The preparation method of metal thermal electrical converter porous silicon carbide titanium electrode material.Butyl titanate is dissolved in dehydrated alcohol by this method,
Stirring, is added dropwise acetic acid, is made for solution A.Nitre acid for adjusting pH is used after dehydrated alcohol is mixed with deionized water, and it is molten that B is made
Liquid.B liquid is added dropwise in A liquid, with nitric acid regulation system pH value, aqueous sucrose solution is added dropwise and obtains the molten of titanium carbide
Glue becomes stable gel after ageing.Gel is dried, is ground, compression moulding, calcines and is cooled to room temperature.It is right
After BASE pipe is surface-treated, using silk screen print method, titanium carbide active electrode material is assembled into surface treated
On BASE tube cathode and anode, porous silicon carbide Ti electrode is obtained finally by heating BASE pipe.Preparation process of the present invention does not use
Hydrogen simplifies preparation method, reduces preparation cost, safely preparing for high-volume coating material may be implemented.
A kind of the technical solution adopted by the present invention to solve the technical problems: Alkali metal thermoelectric converter porous silicon carbide titanium electricity
The preparation method of pole material, its main feature is that the following steps are included:
Step 1: titanium source and carbon source are taken in the following proportions, and butyl titanate: acetic acid: molar ratio=1:2 of deionized water:
5, butyl titanate: molar ratio=1:4 of volume ratio=1:4 of dehydrated alcohol, Ti:C.Butyl titanate is dissolved in 2/ at room temperature
It in the dehydrated alcohol of 3 amounts and stirs, stirring rate 50-100r/min forms the alcoholic solution of titanium, dropwise by the acetic acid of calculation amount
It is added in the alcoholic solution of titanium, forms solution A；It is used after the dehydrated alcohol of remaining 1/3 amount is mixed with the deionized water of calculation amount
Nitre acid for adjusting pH value forms B solution to 2.0-4.0.
Step 2: B solution is added dropwise in solution A, drop rate is about 0.2-0.7mL/min.B solution drips
Later with nitre acid for adjusting pH value to 2.0-4.0, then aqueous sucrose solution is added dropwise to the colloidal sol to form titanium carbide, after colloidal sol ageing
As stable gel.
Step 3: gel is dry under the conditions of 70-100 DEG C, drying time 18-36h grinds simultaneously compression moulding, it
It is calcined under the conditions of vacuum degree is 10-15Pa afterwards, calcination temperature is 1200-1500 DEG C, and heating rate is 8-15 DEG C/min, heat preservation
Time is 4-8h, is then cooled down, and cooling carries out under argon atmosphere.
Step 4: BASE pipe is carried out at surface roughness with 400 mesh, 800 mesh, 1200 mesh and 2000 mesh sand paper respectively
Reason, by treated, BASE pipe is ultrasonic in ethanol, and ultrasonic time 1-3min is placed into drying box and dried, drying temperature
It is 70-100 DEG C.
Step 5: weigh mass percent be 80% carbonized titanium powder, 10% bisphenol A type epoxy resin, 2% acid anhydrides
Class curing agent, 0.5% methylimidazole promotor, 5% butyl acetate, 1.5% reactive diluent 692,0.5% metatitanic acid
Tetra-ethyl ester and 0.5% polyamide wax stir evenly, and form slurry.
By the printing net of attachment and secured 300 mesh on the outside of BASE pipe, then slurry is uniformly brushed with scraper outer in BASE pipe
Surface.BASE pipe is stood into 10-15min in air, is dried at 70-100 DEG C.
By the printing net of attachment and secured 300 mesh on the inside of BASE pipe, then slurry is uniformly brushed with fine, soft fur pen and is managed in BASE
Inner surface.BASE pipe is stood into 10-15min in air, is dried at 70-100 DEG C.
It is vacuumized Step 6: the BASE pipe for having assembled titanium carbide active electrode material is placed in rubber sleeve, Zhi Houfang
Enter the chamber indoor pressurization of isostatic pressing machine, the cavity indoor pressure of isostatic pressing machine is 10-100MPa, and BASE pipe is finally placed in 140-
20-25min is kept the temperature in 170 DEG C of tube furnaces, the N being passed through with the speed of 300-320mL/min2, 1- is kept the temperature at 800-1000 DEG C
2h, heating rate are 1-8 DEG C/min.
The beneficial effects of the present invention are: butyl titanate is dissolved in dehydrated alcohol by this method, vinegar is added dropwise in stirring
Acid is made for solution A.Nitre acid for adjusting pH is used after dehydrated alcohol is mixed with deionized water, and B solution is made.B liquid is added dropwise
Into A liquid, with nitric acid regulation system pH value, aqueous sucrose solution is added dropwise and obtains the colloidal sol of titanium carbide, becomes after ageing and stablize
Gel.Gel is dried, is ground, compression moulding, calcines and is cooled to room temperature.BASE pipe is surface-treated
Afterwards, using silk screen print method, titanium carbide active electrode material is assembled on surface treated BASE tube cathode and anode,
Porous silicon carbide Ti electrode is obtained finally by heating BASE pipe.Preparation process of the present invention do not use hydrogen, simplify preparation method,
It reduces preparation cost, safely preparing for high-volume coating material may be implemented.
It elaborates with reference to the accompanying drawings and detailed description to the present invention.
Detailed description of the invention
Fig. 1 is the XRD diagram picture of titanium carbide powder prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM image of titanium carbide powder prepared by the embodiment of the present invention 1.
Fig. 3 is the thickness schematic diagram for the TiC film that the embodiment of the present invention 1 is prepared under different printing speed.
Fig. 4 is the binding force song of the titanium carbide films material measurement prepared using scratching instrument to the embodiment of the present invention 1~4
Line.
Fig. 5 is the nitrogen adsorption desorption loop line of titanium carbide material prepared by the embodiment of the present invention 1~3.
Specific embodiment
Following embodiment referring to Fig.1-5.
Embodiment 1:
(1) 15mL butyl titanate, 40mL dehydrated alcohol, 5mL acetic acid are measured, is at room temperature dissolved in butyl titanate anhydrous
It in ethyl alcohol and stirs, mixing speed 80r/min adds and acetic acid is added dropwise in mixed liquor, obtains solution A.It measures
20mL dehydrated alcohol, 4mL deionized water, with nitre acid for adjusting pH value to 3.0 after mixing, this is B liquid.
(2) B liquid is added dropwise in A liquid, drop rate is about 0.5mL/min.B drop is adjusted after adding with nitric acid
The colloidal sol in system up to titanium carbide is added dropwise to 2.5, then by aqueous sucrose solution in system pH, becomes after colloidal sol ageing and stablizes
Gel.
It is (3) gel obtained in above-mentioned steps is dry at 80 DEG C to grind and be pressed into the shape of 10mm × 2mm for 24 hours,
Calcine under vacuum conditions again, temperature be 1500 DEG C, heating rate be 10 DEG C/min, soaking time 5h, vacuum degree 10Pa,
Finally cool down, when cooling carries out under argon atmosphere.
(4) first unified 400 mesh, 800 mesh, 1200 mesh, 2000 mesh sand paper handle BASE pipe surface.It is thick to prepare surface
The uniform BASE pipe of rugosity, is subsequently placed into ultrasound 2min in alcohol, places into 85 DEG C of drying boxes and dry.
(5) 16g carbonized titanium powder, 2g bisphenol A type epoxy resin, 0.4g acid anhydride type curing agent 0.1g methylimidazole is weighed to promote
Agent, 1g butyl acetate (non-activated thinner), 0.3g reactive diluent 692,0.1g tetraethyl titanate (adhesive force is urged into agent),
0.1g polyamide wax (sagging inhibitor) stirs in beaker, stirs evenly up to slurry.
The printing net of attachment and secured 300 mesh on the outside of BASE pipe, then takes appropriate slurry on printing net, after use scraper
In certain direction by slurry uniform brush in BASE tube outer surface.Static 10min in air.It is subsequently placed in 80 DEG C of baking oven
It is dried.
The printing net of attachment and secured 300 mesh on the inside of BASE pipe, then dips appropriate slurry with fine, soft fur pen, after by fine, soft fur
Pen protrudes on the inside of BASE pipe, according to certain orientation by slurry uniform brush in BASE pipe internal surface.Static 10min in air.
It is subsequently placed in 80 DEG C of baking oven and is dried.
(6) BASE pipe is placed on after being vacuumized in rubber sleeve and is put into the chamber of isostatic pressing machine, pressure 30MPa.Most
Afterwards, BASE pipe is placed in tube furnace and is heated to 150 DEG C of heat preservation 20min, after N is passed through with the speed of 300ml/min2Continue to heat
To 800 DEG C of heat preservation 2h, heating rate is 1 DEG C/min.Active material is prepared on the porous anode and cathode of BASE pipe by this.
From figure 1 it appears that TiO2 disappears, titanium carbide peak is sharp, and the crystallization degree of titanium carbide films is good.From Fig. 2
It can be seen that the particle diameter distribution of material is probably at 1-3 μm.And the film thickness formed in the case where most thin is 4 μm, illustrates particle
Size even be not enough to influence the thickness of film.As can be seen from Figure 3 silk-screen printing one time when, the thickness of film is less than 5 μm.
As can be seen from Figure 4 with the increase of heating rate, binding force gradually weakens.As can be seen from Figure 5 with heating rate
Increase, electrode gap rate reduce.
Embodiment 2:
(1) 15mL butyl titanate, 40mL dehydrated alcohol, 5mL acetic acid are measured, is at room temperature dissolved in butyl titanate anhydrous
It in ethyl alcohol and stirs, mixing speed 100r/min adds and acetic acid is added dropwise in mixed liquor, obtains solution A.It measures
20mL dehydrated alcohol, 4mL deionized water, with nitre acid for adjusting pH value to 4.0 after mixing, this is B liquid.
(2) B liquid is added dropwise in A liquid, drop rate is about 0.7mL/min.B drop is adjusted after adding with nitric acid
The colloidal sol in system up to titanium carbide is added dropwise to 4.0, then by aqueous sucrose solution in system pH, becomes after colloidal sol ageing and stablizes
Gel.
(3) gel obtained in above-mentioned steps is dried to 18h at 100 DEG C, grinds and be pressed into the shape of 10mm × 2mm
Shape, then calcine under vacuum conditions, temperature are 1200 DEG C, and heating rate is 15 DEG C/min, soaking time 4h, and vacuum degree is
15Pa finally cools down, and when cooling carries out under argon atmosphere.
(4) first unified 400 mesh, 800 mesh, 1200 mesh, 2000 mesh sand paper handle BASE pipe surface.It is thick to prepare surface
The uniform BASE pipe of rugosity, is subsequently placed into ultrasound 3min in alcohol, places into 100 DEG C of drying boxes and dry.
(5) 16g carbonized titanium powder, 2g bisphenol A type epoxy resin, 0.4g acid anhydride type curing agent 0.1g methylimidazole is weighed to promote
Agent, 1g butyl acetate (non-activated thinner), 0.3g reactive diluent 692,0.1g tetraethyl titanate (adhesive force is urged into agent),
0.1g polyamide wax (sagging inhibitor) stirs in beaker, stirs evenly up to slurry.
The printing net of attachment and secured 300 mesh on the outside of BASE pipe, then takes appropriate slurry on printing net, after use scraper
In certain direction by slurry uniform brush in BASE tube outer surface.Static 15min in air.It is subsequently placed in 100 DEG C of baking oven
In be dried.
The printing net of attachment and secured 300 mesh on the inside of BASE pipe, then dips appropriate slurry with fine, soft fur pen, after by fine, soft fur
Pen protrudes on the inside of BASE pipe, according to certain orientation by slurry uniform brush in BASE pipe internal surface.Static 15min in air.
It is subsequently placed in 100 DEG C of baking oven and is dried.
(6) BASE pipe is placed on after being vacuumized in rubber sleeve and is put into the chamber of isostatic pressing machine, pressure 100MPa.Most
Afterwards, BASE pipe is placed in tube furnace and is heated to 170 DEG C of heat preservation 25min, after N is passed through with the speed of 320ml/min2Continue to heat
To 1000 DEG C of heat preservation 1h, heating rate is 3 DEG C/min.This is prepared into to the porous anode and cathode of BASE pipe for active material
On.
As can be seen from Figure 4 with the increase of heating rate, binding force gradually weakens.As can be seen from Figure 5 with
The increase of heating rate, electrode gap rate reduce.
Embodiment 3:
(1) 15mL butyl titanate, 40mL dehydrated alcohol, 5mL acetic acid are measured, is at room temperature dissolved in butyl titanate anhydrous
It in ethyl alcohol and stirs, mixing speed 90r/min adds and acetic acid is added dropwise in mixed liquor, obtains solution A.It measures
20mL dehydrated alcohol, 4mL deionized water, with nitre acid for adjusting pH value to 2.0 after mixing, this is B liquid.
(2) B liquid is added dropwise in A liquid, drop rate is about 0.2mL/min.B drop is adjusted after adding with nitric acid
The colloidal sol in system up to titanium carbide is added dropwise to 3.0, then by aqueous sucrose solution in system pH, becomes after colloidal sol ageing and stablizes
Gel.
(3) gel obtained in above-mentioned steps is dried to 36h at 90 DEG C, grinds and be pressed into the shape of 10mm × 2mm,
Calcine under vacuum conditions again, temperature be 1400 DEG C, heating rate be 8 DEG C/min, soaking time 6h, vacuum degree 10Pa,
Finally cool down, when cooling carries out under argon atmosphere.
(4) first unified 400 mesh, 800 mesh, 1200 mesh, 2000 mesh sand paper handle BASE pipe surface.It is thick to prepare surface
The uniform BASE pipe of rugosity, is subsequently placed into ultrasound 2min in alcohol, places into 90 DEG C of drying boxes and dry.
(5) 16g carbonized titanium powder, 2g bisphenol A type epoxy resin, 0.4g acid anhydride type curing agent 0.1g methylimidazole is weighed to promote
Agent, 1g butyl acetate (non-activated thinner), 0.3g reactive diluent 692,0.1g tetraethyl titanate (adhesive force is urged into agent),
0.1g polyamide wax (sagging inhibitor) stirs in beaker, stirs evenly up to slurry.
The printing net of attachment and secured 300 mesh on the outside of BASE pipe, then takes appropriate slurry on printing net, after use scraper
In certain direction by slurry uniform brush in BASE tube outer surface.Static 12min in air.It is subsequently placed in 80 DEG C of baking oven
It is dried.
The printing net of attachment and secured 300 mesh on the inside of BASE pipe, then dips appropriate slurry with fine, soft fur pen, after by fine, soft fur
Pen protrudes on the inside of BASE pipe, according to certain orientation by slurry uniform brush in BASE pipe internal surface.Static 12min in air.
It is subsequently placed in 80 DEG C of baking oven and is dried.
(6) BASE pipe is placed on after being vacuumized in rubber sleeve and is put into the chamber of isostatic pressing machine, pressure 10MPa.Most
Afterwards, BASE pipe is placed in tube furnace and is heated to 140 DEG C of heat preservation 20min, after N is passed through with the speed of 310ml/min2Continue to heat
To 800 DEG C of heat preservation 1h, heating rate is 5 DEG C/min.Active material is prepared on the porous anode and cathode of BASE pipe by this.
As can be seen from Figure 4 with the increase of heating rate, binding force gradually weakens.As can be seen from Figure 5 with
The increase of heating rate, electrode gap rate reduce.
Embodiment 4:
(1) 15mL butyl titanate, 40mL dehydrated alcohol, 5mL acetic acid are measured, is at room temperature dissolved in butyl titanate anhydrous
It in ethyl alcohol and stirs, mixing speed 50r/min adds and acetic acid is added dropwise in mixed liquor, obtains solution A.It measures
20mL dehydrated alcohol, 4mL deionized water, with nitre acid for adjusting pH value to 4.0 after mixing, this is B liquid.
(2) B liquid is added dropwise in A liquid, drop rate is about 0.4mL/min.B drop is adjusted after adding with nitric acid
The colloidal sol in system up to titanium carbide is added dropwise to 2.0, then by aqueous sucrose solution in system pH, becomes after colloidal sol ageing and stablizes
Gel.
(3) gel obtained in above-mentioned steps is dried to 21h at 70 DEG C, grinds and be pressed into the shape of 10mm × 2mm,
Calcine under vacuum conditions again, temperature be 1300 DEG C, heating rate be 9 DEG C/min, soaking time 7h, vacuum degree 13Pa,
Finally cool down, when cooling carries out under argon atmosphere.
(4) first unified 400 mesh, 800 mesh, 1200 mesh, 2000 mesh sand paper handle BASE pipe surface.It is thick to prepare surface
The uniform BASE pipe of rugosity, is subsequently placed into ultrasound 1min in alcohol, places into 70 DEG C of drying boxes and dry.
(5) 16g carbonized titanium powder, 2g bisphenol A type epoxy resin, 0.4g acid anhydride type curing agent 0.1g methylimidazole is weighed to promote
Agent, 1g butyl acetate (non-activated thinner), 0.3g reactive diluent 692,0.1g tetraethyl titanate (adhesive force is urged into agent),
0.1g polyamide wax (sagging inhibitor) stirs in beaker, stirs evenly up to slurry.
The printing net of attachment and secured 300 mesh on the outside of BASE pipe, then takes appropriate slurry on printing net, after use scraper
In certain direction by slurry uniform brush in BASE tube outer surface.Static 13min in air.It is subsequently placed in 70 DEG C of baking oven
It is dried.
The printing net of attachment and secured 300 mesh on the inside of BASE pipe, then dips appropriate slurry with fine, soft fur pen, after by fine, soft fur
Pen protrudes on the inside of BASE pipe, according to certain orientation by slurry uniform brush in BASE pipe internal surface.Static 13min in air.
It is subsequently placed in 70 DEG C of baking oven and is dried.
(6) BASE pipe is placed on after being vacuumized in rubber sleeve and is put into the chamber of isostatic pressing machine, pressure 70MPa.Most
Afterwards, BASE pipe is placed in tube furnace and is heated to 160 DEG C of heat preservation 21min, after N is passed through with the speed of 300ml/min2Continue to heat
To 900 DEG C of heat preservation 1.5h, heating rate is 8 DEG C/min.This is prepared into to the porous anode and cathode of BASE pipe for active material
On.
As can be seen from Figure 4 with the increase of heating rate, binding force gradually weakens.
Claims (1)
1. a kind of preparation method of Alkali metal thermoelectric converter porous silicon carbide titanium electrode material, it is characterised in that including following step
It is rapid:
Step 1: titanium source and carbon source are taken in the following proportions, butyl titanate: acetic acid: molar ratio=1:2:5 of deionized water, titanium
Sour four butyl esters: molar ratio=1:4 of volume ratio=1:4 of dehydrated alcohol, Ti:C；Butyl titanate is dissolved in 2/3 amount at room temperature
Dehydrated alcohol in and stir, stirring rate 50-100r/min forms the alcoholic solution of titanium, and the acetic acid of calculation amount is added dropwise
Enter into the alcoholic solution of titanium, forms solution A；Nitre is used after the dehydrated alcohol of remaining 1/3 amount is mixed with the deionized water of calculation amount
Acid for adjusting pH value forms B solution to 2.0-4.0；
Step 2: B solution is added dropwise in solution A, drop rate is about 0.2-0.7mL/min；After B solution drips
With nitre acid for adjusting pH value to 2.0-4.0, then aqueous sucrose solution is added dropwise to the colloidal sol to form titanium carbide, become after colloidal sol ageing
Stable gel；
Step 3: gel is dry under the conditions of 70-100 DEG C, drying time 18-36h grinds simultaneously compression moulding, Zhi Hou
Vacuum degree is calcined under the conditions of being 10-15Pa, and calcination temperature is 1200-1500 DEG C, and heating rate is 8-15 DEG C/min, soaking time
For 4-8h, then cool down, cooling carries out under argon atmosphere；
Step 4: BASE pipe is subjected to surface roughness processing with 400 mesh, 800 mesh, 1200 mesh and 2000 mesh sand paper respectively, it will
Treated, and BASE pipe is ultrasonic in ethanol, and ultrasonic time 1-3min is placed into drying box and dried, drying temperature 70-
100℃；
Step 5: weigh mass percent be 80% carbonized titanium powder, 10% bisphenol A type epoxy resin, 2% anhydride it is solid
Agent, 0.5% methylimidazole promotor, 5% butyl acetate, 1.5% reactive diluent 692,0.5% metatitanic acid tetrem
Ester and 0.5% polyamide wax stir evenly, and form slurry；
By the printing net of attachment and secured 300 mesh on the outside of BASE pipe, then slurry is uniformly brushed in BASE tube outer surface with scraper；
BASE pipe is stood into 10-15min in air, is dried at 70-100 DEG C；
By the printing net of attachment and secured 300 mesh on the inside of BASE pipe, then slurry is uniformly brushed to the table in BASE is managed with fine, soft fur pen
Face；BASE pipe is stood into 10-15min in air, is dried at 70-100 DEG C；
It vacuumizes Step 6: the BASE pipe for having assembled titanium carbide active electrode material is placed in rubber sleeve, is put into later
The cavity indoor pressure of the chamber indoor pressurization of static pressure machine, isostatic pressing machine is 10-100MPa, and BASE pipe is finally placed in 140-170 DEG C
20-25min is kept the temperature in tube furnace, the N being passed through with the speed of 300-320mL/min2, 1-2h is kept the temperature at 800-1000 DEG C, is risen
Warm speed is 1-8 DEG C/min.
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| CN111892420A (en) * | 2020-07-29 | 2020-11-06 | 南京工业大学 | Method for preparing massive titanium carbide, titanium nitride or titanium carbonitride aerogel |
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