Summary of the invention
In order to overcome the raw materials used deficiency that is restricted to soluble inorganic salt that can be expensive of prior art, the invention provides a kind of preparation method of titanate powder, raw materials used is insoluble oxide compound or the insoluble salt that nature extensively exists, can widen the raw material sources of hydrothermal preparation ceramic powder, make preparation cost reduce.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparing titanate ferroelectric powder, it is characterized in that, and comprise the steps:
1) be PbTiO with chemical pure plumbous oxide, chemical pure titanium oxide by stoichiometric ratio
3Batching; Chemical pure bismuthous oxide bismuth trioxide, chemical pure titanium oxide are Bi by chemical dosage ratio
4Ti
3O
12Batching; Chemical pure barium carbonate, chemical pure titanium oxide are BaTiO by chemical dosage ratio
3Batching; Chemical pure Strontium carbonate powder, chemical pure titanium oxide are pressed chemical dosage ratio SrTiO
3Batching, the potassium hydroxide of weighing chemical pure then is as mineralizer, and mineralizer concentration is 3~7ml/L;
2) the pairing raw material of the titanate that will prepare is poured in the heating kettle, and the compactedness according to 80% adds deionized water, mixes;
3) begin to be heated to 140~160 ℃ from room temperature, be incubated and cool to room temperature with the furnace after 8~24 hours with the heating rate of 1~3 ℃/min;
4) take out ready prepared titanate ferroelectric powder, use deionized water rinsing, till the deionized water that cleans is neutrality, seasoning then.
The invention has the beneficial effects as follows, because the insoluble oxide compound or the insoluble salt that adopt nature extensively to exist are raw material, the temperature of reaction of preparation process drops to 140~160 ℃ for 180~200 ℃, simplified technological process, widen the raw material sources of preparation ceramic powder, made preparation cost reduce greatly.
The invention will be further described below in conjunction with drawings and Examples.
Embodiment
Embodiment 1, is PbTiO with chemical pure yellow lead oxide, chemical pure titanium oxide by stoichiometric ratio
3Carry out weigh batching: yellow lead oxide 1.5782g, titanium oxide 0.5649g; According to concentration 3mL/L weighing chemical pure potassium hydroxide 7.1848g.The material for preparing is directly poured in the heating kettle, and its total volume is 55mL.The deionized water that adds 35mL then, the good seal heating kettle.Begin to be heated to 140 ℃ from room temperature then, be incubated 8 hours, cool to room temperature with the furnace with 1 ℃/min.Filter cleaning with deionized water, till the deionized water after cleaning was neutrality, last seasoning was finished product.
Can it is evident that from the stereoscan photograph of Fig. 1: crystal grain presents cubic, and size is even, about 0.5 μ m, and crystal development is complete, and the final product of X diffracting spectrum explanation is the pure perovskite phase structure, and reacting completely of raw material do not have dephasign to occur.
Embodiment 2, are PbTiO with chemical pure yellow lead oxide, chemical pure titanium oxide by stoichiometric ratio
3Carry out weigh batching: yellow lead oxide 1.5782g, titanium oxide 0.5649g; According to concentration 5mL/L weighing chemical pure potassium hydroxide 11.9747g.The material for preparing is directly poured in the heating kettle, and its total volume is 55mL.The deionized water that adds 35mL then, the good seal heating kettle.Begin to be heated to 145 ℃ from room temperature then, be incubated 10 hours, cool to room temperature with the furnace with 2 ℃/min.Filter cleaning with deionized water, till the deionized water after cleaning was neutrality, last seasoning was finished product.
Embodiment 3, are PbTiO with chemical pure yellow lead oxide, chemical pure titanium oxide by stoichiometric ratio
3Carry out weigh batching: yellow lead oxide 1.5782g, titanium oxide 0.5649g; According to concentration 3mL/L weighing chemical pure potassium hydroxide 7.1848g.The material for preparing is directly poured in the heating kettle, and its total volume is 55mL.The deionized water that adds 35mL then, the good seal heating kettle.Begin to be heated to 145 ℃ from room temperature then, be incubated 16 hours, cool to room temperature with the furnace with 3 ℃/min.Filter cleaning with deionized water, till the deionized water after cleaning was neutrality, last seasoning was finished product.
Can it is evident that from the stereoscan photograph of Fig. 2: crystal grain presents cubic, and size is even, about 0.8 μ m, and crystal development is complete, and the final product of X diffracting spectrum explanation is the pure perovskite phase structure, and reacting completely of raw material do not have dephasign to occur.
Embodiment 4, are Bi with chemical pure bismuthous oxide bismuth trioxide, chemical pure titanium oxide by stoichiometric ratio
4Ti
3O
12Carry out weigh batching: bismuthous oxide bismuth trioxide 3.3283g, titanium oxide 0.4237g; According to concentration 5mL/L weighing chemical pure potassium hydroxide 11.9747g.The material for preparing is directly poured in the heating kettle, and its total volume is 55mL.The deionized water that adds 35mL then, the good seal heating kettle.Begin to be heated to 150 ℃ from room temperature then, be incubated 16 hours, cool to room temperature with the furnace with 1 ℃/min.Filter cleaning with deionized water, till the deionized water after cleaning was neutrality, last seasoning was finished product.
Can it is evident that from the stereoscan photograph of Fig. 3: crystal grain is in the form of sheets, and is evenly big or small, about 0.8 μ m, and crystal development is complete, and the final product of X diffracting spectrum explanation is the pure perovskite phase structure, and reacting completely of raw material do not have dephasign to occur.
Embodiment 5, are Bi with chemical pure bismuthous oxide bismuth trioxide, chemical pure titanium oxide by stoichiometric ratio
4Ti
3O
12Carry out weigh batching: bismuthous oxide bismuth trioxide 3.3283g, titanium oxide 0.4237g; According to concentration 7mL/L weighing chemical pure potassium hydroxide 16.7646g.The material for preparing is directly poured in the heating kettle, and its total volume is 55mL.The deionized water that adds 35mL then, the good seal heating kettle.Begin to be heated to 150 ℃ from room temperature then, be incubated 14 hours, cool to room temperature with the furnace with 2 ℃/min.Filter cleaning with deionized water, till the deionized water after cleaning was neutrality, last seasoning was finished product.
Embodiment 6, are Bi with chemical pure bismuthous oxide bismuth trioxide, chemical pure titanium oxide by stoichiometric ratio
4Ti
3O
12Carry out weigh batching: bismuthous oxide bismuth trioxide 3.3283g, titanium oxide 0.4237g; According to concentration 3mL/L weighing chemical pure potassium hydroxide 7.1848g.The material for preparing is directly poured in the heating kettle, and its total volume is 55mL.The deionized water that adds 35mL then, the good seal heating kettle.Begin to be heated to 150 ℃ from room temperature then, be incubated 24 hours, cool to room temperature with the furnace with 1 ℃/min.Filter cleaning with deionized water, till the deionized water after cleaning was neutrality, last seasoning was finished product.
Can it is evident that from the stereoscan photograph of Fig. 4: crystal grain is in the form of sheets, and is evenly big or small, about 0.8 μ m, and crystal development is complete, and the final product of X diffracting spectrum explanation is the pure perovskite phase structure, and reacting completely of raw material do not have dephasign to occur.
Embodiment 7, are BaTiO with chemical pure barium carbonate, chemical pure titanium oxide by stoichiometric ratio
3Carry out weigh batching, barium carbonate 1.3953g, titanium oxide 0.5649g; According to concentration 3mL/L weighing chemical pure potassium hydroxide 7.1848g.The material for preparing is directly poured in the heating kettle, and its total volume is 55mL.The deionized water that adds 35mL then, the good seal heating kettle.Begin to be heated to 153 ℃ from room temperature then, be incubated 16 hours, cool to room temperature with the furnace with 1 ℃/min.Filter cleaning with deionized water, till the deionized water after cleaning was neutrality, last seasoning was finished product.
Embodiment 8, are BaTiO with chemical pure barium carbonate, chemical pure titanium oxide by stoichiometric ratio
3Carry out weigh batching, barium carbonate 1.3953g, titanium oxide 0.5649g; According to concentration 7mL/L weighing chemical pure potassium hydroxide 16.7646g.The material for preparing is directly poured in the heating kettle, and its total volume is 55mL.The deionized water that adds 35mL then, the good seal heating kettle.Begin to be heated to 150 ℃ from room temperature then, be incubated 16 hours, cool to room temperature with the furnace with 1 ℃/min.Filter cleaning with deionized water, till the deionized water after cleaning was neutrality, last seasoning was finished product.
Embodiment 9, are SrTiO with chemical pure Strontium carbonate powder, chemical pure titanium oxide by stoichiometric ratio
3Carry out weigh batching, Strontium carbonate powder 1.0545g, titanium oxide 0.5649g; According to concentration 5mL/L weighing chemical pure potassium hydroxide 11.9747g.The material for preparing is directly poured in the heating kettle, and its total volume is 55mL.The deionized water that adds 35mL then, the good seal heating kettle.Begin to be heated to 155 ℃ from room temperature then, be incubated 16 hours, cool to room temperature with the furnace with 1 ℃/min.Filter cleaning with deionized water, till the deionized water after cleaning was neutrality, last seasoning was finished product.
Embodiment 10, are SrTiO with chemical pure Strontium carbonate powder, chemical pure titanium oxide by stoichiometric ratio
3Carry out weigh batching, Strontium carbonate powder 1.0545g, titanium oxide 0.5649g; According to concentration 7mL/L weighing chemical pure potassium hydroxide 16.7646g.The material for preparing is directly poured in the heating kettle, and its total volume is 55mL.The deionized water that adds 35mL then, the good seal heating kettle.Begin to be heated to 160 ℃ from room temperature then, be incubated 16 hours, cool to room temperature with the furnace with 1 ℃/min.Filter cleaning with deionized water, till the deionized water after cleaning was neutrality, last seasoning was finished product.
In a word, insoluble oxide compound or insoluble salt that the present invention adopts nature extensively to exist are raw material, have finished the preparation of titanate by hydrothermal method under 140~160 ℃ low temperature, have widened the raw material sources of preparation titanate powder, reduce cost, realized preparation of industrialization.