CN103787409B - Ti 3o 5raw powder's production technology - Google Patents

Ti 3o 5raw powder's production technology Download PDF

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CN103787409B
CN103787409B CN201410013146.XA CN201410013146A CN103787409B CN 103787409 B CN103787409 B CN 103787409B CN 201410013146 A CN201410013146 A CN 201410013146A CN 103787409 B CN103787409 B CN 103787409B
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powder
raw material
sintering
raw
mixed
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CN103787409A (en
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刘颖
叶金文
张晓燕
朱瑞杰
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Sichuan University
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Sichuan University
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Abstract

Ti 3o 5raw powder's production technology, method one: (1) prepares burden; (2) ball milling makes raw material mix and dry sintering mixed powder; (3) sintering mixed powder is sintered 1 ~ 4 hour in 1000 ~ 1400 DEG C under vacuum or nitrogen or argon gas atmosphere.Method two: (1) prepares burden; (2) ball milling, in ratio of grinding media to material (8 ~ 40): 1, dry grind 2 ~ 6 hours under drum's speed of rotation 100 ~ 300r/min, sieving separating goes out to grind spheroid and namely obtains mixed powder; (3) mixed powder is sintered 1 ~ 4 hour in 700 DEG C ~ 1000 DEG C under vacuum or nitrogen or argon gas atmosphere.Method three: (1) prepares burden; (2) raw material distilled water or deionized water are mixed with mixed solution, use spray-drier mist projection granulating, and dry; (3) by pellet under vacuum or nitrogen or argon gas atmosphere, in 1000 ~ 1400 DEG C sintering 1 ~ 4 hour.The method of the invention can not only obtain high purity Ti 3o 5powder, and energy Simplified flowsheet, reduce costs, realize mass industrialized production.

Description

Ti 3o 5raw powder's production technology
Technical field
The invention belongs to electro-conductive material and gas sensitive technical field, particularly oxygen-sensitive material Ti 3o 5raw powder's production technology.
Background technology
Ti 3o 5as the one in sub-titania meterial, because its special crystalline structure has certain electroconductibility and gas sensitive resistors, this makes it in gas sensitive element device, have good application prospect.As a kind of brand-new material, become one of focus of functional materials research at present.Existing Ti 3o 5preparation method comprise sputtering method, reduction method etc., but the aforesaid method complex operation in bibliographical information, output is little, the demand of laboratory study can only be met, can not suitability for industrialized production, and due to sub-titanium oxide lattice parameter close, aforesaid method is difficult to prepare high purity Ti 3o 5, in product, be usually attended by other sub-titanium oxide impurity in products.And the existence of these impurity must affect Ti 3o 5characteristic, limits its application.Though studies have reported that in the recent period adopting hydrogen to reduce titanium dioxide in molybdenum pipe furnace prepares highly purified Ti 3o 5powder (λ-Ti 3o 5the preparation of powder and the research of optical storage performance thereof, Journal of Inorganic Materials, 2013,28:425-430), but because hydrogen reduction can only reduce the raw material powder contacted with hydrogen, raw material powder can only very thin accumulation one deck, and thus output is also minimum, and hydrogen reduction simultaneously needs a large amount of hydrogen source, cost is high, and hydrogen process complicated operation, have very large insecurity, these all cause very difficult industrialized a large amount of production Ti 3o 5powder, thus the deficiencies in the prior art limit Ti 3o 5apply.
Summary of the invention
The object of the invention is to, for the deficiencies in the prior art, provide Ti 3o 5raw powder's production technology, with Simplified flowsheet, reduces costs, and realizes mass industrialized production high purity Ti 3o 5powder.
Ti provided by the invention 3o 5the first preparation method of powder, processing step is as follows successively:
(1) prepare burden
Raw material is TiO 2powder, carbonaceous reducing agent or titanium matter reductive agent, according to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material;
(2) batch mixing is with dry
The raw material that step (1) measures is put into ball mill and carries out wet-milling dispersion, raw material is mixed (add-on of wet grinding media is limited to flood described raw material and to grind spheroid), then sieving separating goes out to grind spheroid and obtains mixed slurry, described mixed slurry is carried out dry sintering mixed powder;
(3) sinter
Sintering mixed powder prepared by step (2) under vacuum or nitrogen or argon gas atmosphere in 1000 DEG C ~ 1400 DEG C sintering 1 hour ~ 4 hours, continue after cool to less than 100 DEG C with the furnace and come out of the stove, namely obtain Ti 3o 5powder.
The first preparation method above-mentioned, described carbonaceous reducing agent is any one in carbon powder, Graphite Powder 99, activity charcoal powder, wood charcoal powder, glucose; Described titanium matter reductive agent is titanium valve or titanium hydride powder.
The first preparation method above-mentioned, in step (2), the wet grinding media of wet-milling dispersion is any one in deionized water, alcohol, acetone.
The first preparation method above-mentioned, the drying temperature of mixed slurry described in step (2) is 50 DEG C ~ 100 DEG C, and time of drying is 2 hours ~ 6 hours.
Ti provided by the invention 3o 5the second preparation method of powder, processing step is as follows successively:
(1) prepare burden
Raw material is TiO 2powder, carbonaceous reducing agent or titanium matter reductive agent, according to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material;
(2) ball milling
The raw material that step (1) measures is put into high energy ball mill, in ratio of grinding media to material (8 ~ 40): 1, dry grind 2 hours ~ 6 hours under drum's speed of rotation 100r/min ~ 300r/min, sieving separating goes out to grind spheroid and namely obtains mixed powder, and described ratio of grinding media to material refers to the mass ratio of ball-milling medium (grinding element) and polished material (each raw material);
(3) sinter
Mixed powder prepared by step (2) under vacuum or nitrogen or argon gas atmosphere in 700 DEG C ~ 1000 DEG C sintering 1 hour ~ 4 hours, continue after cool to less than 100 DEG C with the furnace and come out of the stove, namely obtain Ti 3o 5powder.
Above-mentioned the second preparation method, described carbonaceous reducing agent is any one in Graphite Powder 99, carbon powder, activity charcoal powder, wood charcoal powder; Described titanium matter reductive agent is titanium valve.
Ti provided by the invention 3o 5the third preparation method of powder, processing step is as follows successively:
Processing step is as follows successively:
(1) prepare burden
Raw material is titanium source and carbonaceous reducing agent, according to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material;
(2) pellet is prepared
Each raw material distilled water step (1) measured or deionized water are mixed with mixed solution, the weight of distilled water or deionized water is (2 ~ 4) with the ratio of each raw material gross weight: 1, then use spray-drier mist projection granulating, and gained pellet is calcined at least 30 minutes in 300 DEG C ~ 600 DEG C under argon shield;
(3) sinter
Pellet prepared by step (2) under vacuum or nitrogen or argon gas atmosphere, in 1000 DEG C ~ 1400 DEG C sintering 1 hour ~ 4 hours, continue after cool to less than 100 DEG C with the furnace and come out of the stove, namely obtain Ti 3o 5powder.
The third preparation method above-mentioned, described titanium source is H 2tiO 3powder or TiOSO 4powder; Described carbonaceous reducing agent is any one in glucose, sucrose, flour, carbon powder.
The third preparation method above-mentioned, in step (2), during mist projection granulating, the temperature out of spray-drier is 180 DEG C ~ 250 DEG C.
Compared with prior art, the present invention has following beneficial effect:
1, the method for the invention technique is simple, low cost of manufacture, and raw material is easy to obtain, production efficiency and security high, thus can realize Ti 3o 5the industrialization scale operation of powder.
2, the method for the invention has prepared the high purity Ti of uniform particle sizes 3o 5powder, ensure that this Ti 3o 5the characteristic of powder, to be applicable to the application of all respects.
Accompanying drawing explanation
Fig. 1 is Ti prepared by embodiment 1 3o 5the stereoscan photograph of powder.
Fig. 2 is Ti prepared by embodiment 1 3o 5the X-ray diffractogram of powder.
Fig. 3 is Ti prepared by embodiment 1 3o 5powder is at the gas sensitive resistors figure of the oxygen atmosphere of concentration 285ppm.
Fig. 4 is Ti prepared by embodiment 11 3o 5the X-ray diffractogram of powder.
Fig. 5 is Ti prepared by embodiment 20 3o 5the stereoscan photograph of powder.
Fig. 6 is Ti prepared by embodiment 20 3o 5the X-ray diffractogram of powder.
Embodiment
Below by specific embodiment to Ti of the present invention 3o 5raw powder's production technology is described further.
Ti prepared by following each embodiment 3o 5the gas sensitive resistors of powder adopts gas sensor material detection system to test, and specific conductivity adopts four-point probe to test.Ratio of grinding media to material refers to the mass ratio of ball-milling medium (grinding element) and polished material.
In following embodiment, described material powder all can be bought from market.
Embodiment 1
In the present embodiment, the first preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron TiO 2powder 88.80wt%,
Micron titanium hydride powder 11.20wt%;
(2) batch mixing is with dry
The raw material that step (1) measures is put into tumbling ball mill, with diameter be φ 10mm WC-8wt%Co sintered carbide ball be grinding spheroid, ratio of grinding media to material is 8:1, with mass concentration 75% alcohol for wet grinding media, its add-on is limited to flood described raw material and to grind spheroid, the lower grinding distribution of rotational speed of ball-mill 30 revs/min 75 hours, raw material is mixed, then sieving separating goes out to grind spheroid and obtains mixed slurry, described mixed slurry to be placed in baking oven at 50 DEG C dry 6 hours to obtain sintering raw mix;
(3) sinter
Sintering raw mix prepared by step (2) is put into pipe type sintering furnace, under the flowing argon gas atmosphere of 200ml/min, is warming up to 1400 DEG C of sintering 1 hour, then cools to room temperature with the furnace, obtain Ti 3o 5powder, its stereoscan photograph is shown in Fig. 1, and X-ray diffractogram is shown in Fig. 2, Ti 3o 5powder is shown in Fig. 3 at the gas sensitive resistors figure of the oxygen atmosphere of concentration 285ppm.As can be seen from Figure 1, obtained powder granule particle diameter is 2-4 μm.As can be seen from Figure 2, obtained powder is high purity Ti 3o 5powder, product has gas sensitive resistors as can be seen from Figure 3.After testing, the Ti for preparing of the present embodiment 3o 5the specific conductivity of powder is 260S/cm.
Embodiment 2
In the present embodiment, the first preparation method of the present invention is adopted to prepare Ti 3o 5powder, processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Nano-TiO 2powder 83.60wt%,
Nano-titanium powder 16.40wt%;
(2) batch mixing is with dry
The raw material that step (1) measures is put into tumbling ball mill, with diameter be φ 10mm WC-8wt%Co sintered carbide ball be grinding spheroid, ratio of grinding media to material is 8:1, take deionized water as wet grinding media, its add-on is limited to flood described raw material and to grind spheroid, the lower grinding distribution of rotational speed of ball-mill 40 revs/min 70 hours, raw material is mixed, then sieving separating goes out to grind spheroid and obtains mixed slurry, described mixed slurry to be placed in baking oven at 100 DEG C dry 2 hours to obtain sintering raw mix;
(3) sinter
Sintering raw mix prepared by step (2) is put into pipe type sintering furnace, under the flowing Ar gas atmosphere of 200ml/min, is warming up to 1000 DEG C of sintering 4 hours, then cools to room temperature with the furnace, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 400-800nm, and specific conductivity is 110S/cm.
Embodiment 3
In the present embodiment, the first preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron TiO 2powder 92.42wt%,
Micron charcoal powder 7.58wt%;
(2) batch mixing is with dry
The raw material that step (1) measures is put into tumbling ball mill, with diameter be φ 10mm WC-8wt%Co sintered carbide ball be grinding spheroid, ratio of grinding media to material is 8:1, take acetone as wet grinding media, its add-on, to flood described raw material and grinding spheroid is limited, the lower grinding distribution of rotational speed of ball-mill 30 revs/min 80 hours, makes raw material mix, then sieving separating goes out to grind spheroid and obtains mixed slurry, described mixed slurry to be placed in baking oven at 60 DEG C dry 4 hours to obtain sintering raw mix;
(3) sinter
Sintering raw mix prepared by step (2) is put into vacuum carbon tube furnace, and being evacuated to vacuum tightness is 1 × 10 -1pa, is warming up to 1350 DEG C of sintering 2.5 hours, then cools to room temperature with the furnace, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 2-6 μm, and specific conductivity is 280S/cm.
Embodiment 4
In the present embodiment, the first preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Nano-TiO 2powder 92.42wt%,
Nano carbon black powder 7.58wt%;
(2) batch mixing is with dry
The raw material that step (1) measures is put into tumbling ball mill, with diameter be φ 10mm WC-8wt%Co sintered carbide ball be grinding spheroid, ratio of grinding media to material is 8:1, take dehydrated alcohol as wet grinding media, its add-on, to flood described raw material and grinding spheroid is limited, the lower grinding distribution of rotational speed of ball-mill 20 revs/min 90 hours, makes raw material mix, then sieving separating goes out to grind spheroid and obtains mixed slurry, described mixed slurry to be placed in baking oven at 60 DEG C dry 4 hours to obtain sintering raw mix;
(3) sinter
Sintering raw mix prepared by step (2) is put into vacuum carbon tube furnace, and being evacuated to vacuum tightness is 1 × 10-1Pa, is warming up to 1000 DEG C of sintering 4 hours, then cools to room temperature with the furnace, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 500-800nm, and specific conductivity is 120S/cm.
Embodiment 5
In the present embodiment, the first preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron TiO 2powder 92.42wt%,
Particulate active powdered carbon body 7.58wt%;
(2) batch mixing is with dry
The raw material that step (1) measures is put into tumbling ball mill, with diameter be φ 10mm WC-8wt%Co sintered carbide ball be grinding spheroid, ratio of grinding media to material is 5:1, with mass concentration 75% alcohol for wet grinding media, its add-on is limited to flood described raw material and to grind spheroid, the lower grinding distribution of rotational speed of ball-mill 30 revs/min 72 hours, raw material is mixed, then sieving separating goes out to grind spheroid and obtains mixed slurry, described mixed slurry to be placed in baking oven at 75 DEG C dry 3 hours to obtain sintering raw mix;
(3) sinter
Sintering raw mix prepared by step (2) is put into vacuum carbon tube furnace, and being evacuated to vacuum tightness is 1 × 10-1Pa, is warming up to 1100 DEG C of sintering 4 hours, then cools to room temperature with the furnace, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 3-6 μm, and specific conductivity is 300S/cm.
Embodiment 6
In the present embodiment, the first preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Nano-TiO 2powder 82.99wt%,
Micron glucose powder 17.01wt%;
(2) batch mixing is with dry
The raw material that step (1) measures is put into tumbling ball mill, with diameter be φ 10mm WC-8wt%Co sintered carbide ball be grinding spheroid, ratio of grinding media to material is 8:1, take dehydrated alcohol as wet grinding media, its add-on, to flood described raw material and grinding spheroid is limited, the lower grinding distribution of rotational speed of ball-mill 30 revs/min 90 hours, makes raw material mix, then sieving separating goes out to grind spheroid and obtains mixed slurry, described mixed slurry to be placed in baking oven at 75 DEG C dry 3 hours to obtain sintering raw mix;
(3) sinter
Sintering raw mix prepared by step (2) is put into vacuum carbon tube furnace, and being evacuated to vacuum tightness is 1 × 10-1Pa, is warming up to 1150 DEG C of sintering 3 hours, then cools to room temperature with the furnace, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 600-800nm, and specific conductivity is 125S/cm.
Embodiment 7
In the present embodiment, the first preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron TiO 2powder 92.42wt%,
Micron graphite powder 7.58wt%;
(2) batch mixing is with dry
The raw material that step (1) measures is put into tumbling ball mill, with diameter be φ 10mm WC-8wt%Co sintered carbide ball be grinding spheroid, ratio of grinding media to material is 8:1, take dehydrated alcohol as wet grinding media, its add-on is limited to flood described raw material and to grind spheroid, the lower grinding distribution of rotational speed of ball-mill 30 revs/min 80 hours, raw material is mixed, then sieving separating goes out to grind spheroid and obtains mixed slurry, described mixed slurry to be placed in baking oven at 70 DEG C dry 2.5 hours to obtain sintering raw mix;
(3) sinter
Sintering raw mix prepared by step (2) is put into pipe type sintering furnace, under the flowing Ar atmosphere of 200ml/min, is warming up to 1300 DEG C of sintering 3 hours, then cools to room temperature with the furnace, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 5-7 μm, and specific conductivity is 300S/cm.
Embodiment 8
In the present embodiment, the second preparation method of the present invention is adopted to prepare Ti 3o 5powder, processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Nano-TiO 2powder 83.60wt%,
Nano-titanium powder 16.40wt%;
(2) batch mixing is with dry
The raw material that step (1) measures is put into high energy ball mill, with diameter be φ 10mm WC-8wt%Co sintered carbide ball be grinding spheroid, ratio of grinding media to material 8:1, under rotational speed of ball-mill 100 revs/min dry grind 6 hours, raw material is mixed, and then sieving separating goes out to grind spheroid and obtains compound.
(3) sinter
Compound prepared by step (2) is put into pipe type sintering furnace, under the flowing Ar gas atmosphere of 200ml/min, is warming up to 1000 DEG C of sintering 1 hour, then cools to room temperature with the furnace, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 500-800nm, and specific conductivity is 130S/cm.
Embodiment 9
In the present embodiment, the second preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron TiO 2powder 92.42wt%,
Micron charcoal powder 7.58wt%;
(2) batch mixing is with dry
The raw material that step (1) measures is put into high energy ball mill, with diameter be φ 10mm WC-8wt%Co sintered carbide ball be grinding spheroid, ratio of grinding media to material 40:1, under rotational speed of ball-mill 300 revs/min dry grind 2 hours, raw material is mixed, and then sieving separating goes out to grind spheroid and obtains compound;
(3) sinter
Sintering raw mix prepared by step (2) is put into vacuum carbon tube furnace, at the flowing N of 300ml/min 2under atmosphere, be warming up to 700 DEG C of sintering 4 hours, then cool to room temperature with the furnace, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 2-6 μm, and specific conductivity is 270S/cm.
Embodiment 10
In the present embodiment, the second preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron TiO 2powder 92.42wt%,
Particulate active powdered carbon body 7.58wt%;
(2) batch mixing is with dry
The raw material that step (1) measures is put into high energy ball mill, with diameter be φ 10mm WC-8wt%Co sintered carbide ball be grinding spheroid, ratio of grinding media to material 20:1, under rotational speed of ball-mill 200 revs/min dry grind 4 hours, raw material is mixed, and then sieving separating goes out to grind spheroid and obtains compound;
(3) sinter
Sintering raw mix prepared by step (2) is put into vacuum carbon tube furnace, at the flowing N of 300ml/min 2under atmosphere, be warming up to 900 DEG C of sintering 3 hours, then cool to room temperature with the furnace, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 4-7 μm, and specific conductivity is 320S/cm.
Embodiment 11
In the present embodiment, the second preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Nano-TiO 2powder 92.42wt%,
Nano carbon black powder 7.58wt%;
(2) batch mixing is with dry
The raw material that step (1) measures is put into high energy ball mill, with diameter be φ 10mm WC-8wt%Co sintered carbide ball be grinding spheroid, ratio of grinding media to material 40:1, under rotational speed of ball-mill 300 revs/min dry grind 2 hours, raw material is mixed, and then sieving separating goes out to grind spheroid and obtains compound;
(3) sinter
Sintering raw mix prepared by step (2) is put into vacuum carbon tube furnace, at the flowing N of 300ml/min 2under atmosphere, be warming up to 800 DEG C of sintering 4 hours, then cool to room temperature with the furnace, obtain Ti 3o 5powder, its X-ray diffractogram is shown in Fig. 4, and as can be seen from Figure 4, obtained powder is high purity Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 2-4 μm, and specific conductivity is 240S/cm.
Embodiment 12
In the present embodiment, the second preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron TiO 2powder 92.42wt%,
Micron charcoal powder 7.58wt%;
(2) batch mixing is with dry
The raw material that step (1) measures is put into tumbling ball mill, with diameter be φ 10mm WC-8wt%Co sintered carbide ball be grinding spheroid, ratio of grinding media to material 40:1, under rotational speed of ball-mill 300 revs/min dry grind 2 hours, raw material is mixed, and then sieving separating goes out to grind spheroid and obtains compound;
(3) sinter
Sintering raw mix prepared by step (2) is put into vacuum carbon tube furnace, at the flowing N of 300ml/min 2under atmosphere, be warming up to 700 DEG C of sintering 4 hours, then cool to room temperature with the furnace, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 2-6 μm, and specific conductivity is 270S/cm.
Embodiment 13
In the present embodiment, the second preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron TiO 2powder 92.42wt%,
Micron graphite powder 7.58wt%;
2) batch mixing is with dry
The raw material that step (1) measures is put into high energy ball mill, with diameter be φ 10mm WC-8wt%Co sintered carbide ball be grinding spheroid, ratio of grinding media to material 25:1, under rotational speed of ball-mill 200 revs/min dry grind 5 hours, raw material is mixed, and then sieving separating goes out to grind spheroid and obtains compound;
(3) sinter
Sintering raw mix prepared by step (2) is put into vacuum carbon tube furnace, at the flowing N of 300ml/min 2under atmosphere, be warming up to 900 DEG C of sintering 2.5 hours, then cool to room temperature with the furnace, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 5-8 μm, and specific conductivity is 330S/cm.
Embodiment 14
In the present embodiment, the third preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron H 2tiO 3powder 91.15wt%,
Micron sucrose powder 8.85wt%;
(2) pellet is prepared
Each raw material deionized water step (1) measured is mixed with mixed solution, the weight of deionized water is 2:1 with the ratio of each raw material gross weight, then spray-drier mist projection granulating is used, the temperature out of spray-drier is 250 DEG C, and is calcined 30 minutes in 600 DEG C under argon shield by gained pellet;
(3) sinter
Pellet prepared by step (2) is put into pipe type sintering furnace, at the flowing N of 500ml/min 2under gas atmosphere, in 1000 DEG C of sintering 4 hours, continue after cool to less than 100 DEG C with the furnace and come out of the stove, namely obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 4-6 μm, and specific conductivity is 270S/cm.
Embodiment 15
In the present embodiment, the third preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron H 2tiO 390.73wt%,
Micron glucose powder 9.27wt%;
(2) pellet is prepared
Each raw material distilled water step (1) measured is mixed with mixed solution, the weight of distilled water is 4:1 with the ratio of each raw material gross weight, then use spray-drier mist projection granulating, the temperature out of spray-drier is 230 DEG C, and is calcined 40 minutes in 600 DEG C under argon shield by gained pellet;
(3) sinter
Pellet prepared by step (2) is put into pipe type sintering furnace, under vacuum conditions, in 1400 DEG C of sintering 1 hour, continue after cool to less than 100 DEG C with the furnace and come out of the stove, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 5-8 μm, and specific conductivity is 300S/cm
Embodiment 16
In the present embodiment, the third preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron H 2tiO 3powder 96.07wt%,
Micron carbon black powder 3.93wt%;
(2) pellet is prepared
Each raw material distilled water step (1) measured is mixed with mixed solution, the weight of distilled water is 4:1 with the ratio of each raw material gross weight, then use spray-drier mist projection granulating, the temperature out of spray-drier is 230 DEG C, and is calcined 45 minutes in 300 DEG C under argon shield by gained pellet;
(3) sinter
Pellet prepared by step (2) is put into pipe type sintering furnace, under the flowing Ar gas atmosphere of 500ml/min, in 1300 DEG C of sintering 2 hours, continue after cool to less than 100 DEG C with the furnace and come out of the stove, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 5-8 μm, and specific conductivity is 300S/cm
Embodiment 17
In the present embodiment, the third preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron H 2tiO 3powder 88.37wt%,
Flour 11.63wt%;
(2) pellet is prepared
Each raw material distilled water step (1) measured is mixed with mixed solution, the weight of distilled water is 3:1 with the ratio of each raw material gross weight, then use spray-drier mist projection granulating, the temperature out of spray-drier is 230 DEG C, and is calcined 30 minutes in 500 DEG C under argon shield by gained pellet;
(3) sinter
Pellet prepared by step (2) is put into pipe type sintering furnace, at the flowing N of 400ml/min 2under gas atmosphere, in 1200 DEG C of sintering 3 hours, continue after cool to less than 100 DEG C with the furnace and come out of the stove, obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 5-8 μm, and specific conductivity is 300S/cm
Embodiment 18
In the present embodiment, the third preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron TiOSO 42H 2o powder 95.14wt%,
Glucose powder 4.86wt%;
(2) pellet is prepared
Each raw material deionized water step (1) measured is mixed with mixed solution, the weight of deionized water is 3:1 with the ratio of each raw material gross weight, then spray-drier mist projection granulating is used, the temperature out of spray-drier is 200 DEG C, and is calcined 60 minutes in 500 DEG C under argon shield by gained pellet;
(3) sinter
Pellet prepared by step (2) is put into pipe type sintering furnace, at the flowing N of 300ml/min 2under gas atmosphere, in 1200 DEG C of sintering 2.5 hours, continue after cool to less than 100 DEG C with the furnace and come out of the stove, namely obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 1-5 μm, and specific conductivity is 230S/cm.
Embodiment 19
In the present embodiment, the third preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron TiOSO 42H 2o powder 95.37wt%,
Sucrose powder 4.63wt%;
(2) pellet is prepared
Each raw material deionized water step (1) measured is mixed with mixed solution, the weight of deionized water is 3:1 with the ratio of each raw material gross weight, then spray-drier mist projection granulating is used, the temperature out of spray-drier is 200 DEG C, and is calcined 60 minutes in 500 DEG C under argon shield by gained pellet;
(3) sinter
Pellet prepared by step (2) is put into pipe type sintering furnace, at the flowing N of 300ml/min 2under gas atmosphere, in 1200 DEG C of sintering 2.5 hours, continue after cool to less than 100 DEG C with the furnace and come out of the stove, namely obtain Ti3O 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 2-5 μm, and specific conductivity is 240S/cm.
Embodiment 20
In the present embodiment, the third preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron TiOSO 42H 2o powder 98.00wt%,
Micron carbon black powder 2.00wt%;
(2) pellet is prepared
Each raw material deionized water step (1) measured is mixed with mixed solution, the weight of deionized water is 3:1 with the ratio of each raw material gross weight, then spray-drier mist projection granulating is used, the temperature out of spray-drier is 200 DEG C, and is calcined 60 minutes in 500 DEG C under argon shield by gained pellet;
(3) sinter
Pellet prepared by step (2) is put into pipe type sintering furnace, at the flowing N of 300ml/min 2under gas atmosphere, in 1200 DEG C of sintering 2.5 hours, continue after cool to less than 100 DEG C with the furnace and come out of the stove, namely obtain Ti 3o 5powder, its stereoscan photograph is shown in Fig. 5, and X-ray diffractogram is shown in Fig. 6, and as can be seen from Figure 5, obtained powder granule particle size range is 2-5 μm, and as can be seen from Figure 6, obtained powder is high purity Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and specific conductivity is 260S/cm.
Embodiment 21
In the present embodiment, the third preparation method of the present invention is adopted to prepare Ti 3o 5powder, its processing step is as follows successively:
(1) prepare burden
According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material, the weight percent of each raw material is as follows:
Micron TiOSO 42H 2o powder 93.92wt%,
Flour 6.08wt%;
(2) pellet is prepared
Each raw material that step (1) measures is spent distilled water and is mixed with mixed solution, the weight of deionized water is 3:1 with the ratio of each raw material gross weight, then spray-drier mist projection granulating is used, the temperature out of spray-drier is 200 DEG C, and is calcined 60 minutes in 500 DEG C under argon shield by gained pellet;
(3) sinter
Pellet prepared by step (2) is put into pipe type sintering furnace, under the flowing Ar gas atmosphere of 300ml/min, in 1200 DEG C of sintering 2.5 hours, continue after cool to less than 100 DEG C with the furnace and come out of the stove, namely obtain Ti 3o 5powder, this Ti 3o 5powder has gas sensitive resistors, and particle size range is 4-8 μm, and specific conductivity is 310S/cm.

Claims (6)

1. a Ti 3o 5raw powder's production technology, processing step is as follows successively:
(1) prepare burden
Raw material is TiO 2powder, carbonaceous reducing agent or titanium matter reductive agent, described carbonaceous reducing agent is any one in carbon powder, Graphite Powder 99, activity charcoal powder, wood charcoal powder, glucose, and described titanium matter reductive agent is titanium valve body or titanium hydride powder; According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material;
(2) batch mixing is with dry
The raw material that step (1) measures is put into ball mill and carries out wet-milling dispersion, raw material is mixed, then sieving separating goes out to grind spheroid and obtains mixed slurry, described mixed slurry is carried out dry sintering mixed powder;
(3) sinter
Sintering mixed powder prepared by step (2) under vacuum or nitrogen or argon gas atmosphere in 1000 DEG C ~ 1400 DEG C sintering 1 hour ~ 4 hours, continue after cool to less than 100 DEG C with the furnace and come out of the stove, namely obtain Ti 3o 5powder.
2. Ti according to claim 1 3o 5raw powder's production technology, is characterized in that the wet grinding media of wet-milling dispersion in step (2) is any one in water, alcohol, acetone.
3. Ti according to claim 1 or 2 3o 5raw powder's production technology, it is characterized in that the drying temperature of mixed slurry described in step (2) is 50 DEG C ~ 100 DEG C, time of drying is 2 hours ~ 6 hours.
4. a Ti 3o 5raw powder's production technology, processing step is as follows successively:
(1) prepare burden
Raw material is TiO 2powder, carbonaceous reducing agent or titanium matter reductive agent, described carbonaceous reducing agent is any one in carbon powder, Graphite Powder 99, activity charcoal powder, wood charcoal powder, and described titanium matter reductive agent is titanium valve; According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material;
(2) ball milling
The raw material that step (1) measures is put into high energy ball mill, and in ratio of grinding media to material (8 ~ 40): 1, dry grind 2 hours ~ 6 hours under drum's speed of rotation 100r/min ~ 300r/min, sieving separating goes out to grind spheroid and namely obtains mixed powder;
(3) sinter
Mixed powder prepared by step (2) under vacuum or nitrogen or argon gas atmosphere in 700 DEG C ~ 1000 DEG C sintering 1 hour ~ 4 hours, continue after cool to less than 100 DEG C with the furnace and come out of the stove, namely obtain Ti 3o 5powder.
5. a Ti 3o 5raw powder's production technology, processing step is as follows successively:
(1) prepare burden
Raw material is titanium source and carbonaceous reducing agent, and described titanium source is H 2tiO 3powder or TiOSO 4powder, described carbonaceous reducing agent is any one in glucose, sucrose, flour, carbon powder; According to Ti 3o 5the chemical formula of powder and raw materials used between chemical reaction measure each raw material;
(2) pellet is prepared
Each raw material distilled water step (1) measured or deionized water are mixed with mixed solution, the weight of distilled water or deionized water is (2 ~ 4) with the ratio of each raw material gross weight: 1, then use spray-drier mist projection granulating, and gained pellet is calcined at least 30 minutes in 300 DEG C ~ 600 DEG C under argon shield;
(3) sinter
Pellet prepared by step (2) under vacuum or nitrogen or argon gas atmosphere, in 1300 DEG C ~ 1400 DEG C sintering 1 hour ~ 2 hours, continue after cool to less than 100 DEG C with the furnace and come out of the stove, namely obtain Ti 3o 5powder.
6. Ti according to claim 5 3o 5raw powder's production technology, is characterized in that the temperature out of spray-drier during mist projection granulating in step (2) is 180 DEG C ~ 250 DEG C.
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CN104437449A (en) * 2014-12-09 2015-03-25 黑龙江大学 Preparation method of black titanium dioxide visible light photocatalyst
CN105887182A (en) * 2014-12-15 2016-08-24 盱眙新远光学科技有限公司 Preparation technology of trititanium pentoxide crystal
CN104973622B (en) * 2015-02-12 2017-03-22 四川大学 Preparation method of light-induced phase transition storage powdery material lamda-Ti3O5
CN104925858B (en) * 2015-06-09 2017-03-22 四川大学 Push-type dynamic continuous preparation method and sintering device for titanium black powder
CN104925857A (en) * 2015-06-09 2015-09-23 四川大学 Rotary dynamic continuous preparation method for titanium black powder
CN104986749B (en) * 2015-06-09 2019-07-05 四川大学 My(CxN1-x) powder the continuous preparation method of push type dynamic and sintering equipment
CN105692694B (en) * 2016-02-29 2017-06-13 西安电子科技大学 Ti3O5/TiO2The preparation method of mixed crystal nanofiber
CN106865602B (en) * 2017-03-02 2019-04-23 攀枝花学院 Graphite-titanium suboxide composite material preparation method
CN109110804B (en) * 2018-11-09 2021-01-12 攀枝花学院 High-purity magneli phase titanium suboxide and preparation method thereof
CN109485408A (en) * 2019-01-18 2019-03-19 江苏师范大学 A kind of technique of TiC reduction preparation sheet titanium pentoxide
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