CN108394932A - A kind of preparation method of the submicron order barium carbonate powder of good dispersion - Google Patents
A kind of preparation method of the submicron order barium carbonate powder of good dispersion Download PDFInfo
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- CN108394932A CN108394932A CN201810465894.XA CN201810465894A CN108394932A CN 108394932 A CN108394932 A CN 108394932A CN 201810465894 A CN201810465894 A CN 201810465894A CN 108394932 A CN108394932 A CN 108394932A
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- carbonate powder
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- barium carbonate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to inorganic functional powder body material technical fields, more particularly to a kind of preparation method of the submicron order barium carbonate powder of good dispersion, to solve the reunion weight of barium carbonate powder, surface-active is poor, particle diameter distribution is wide, the powder qualities problem such as uniformity and poor fluidity, this method prepares barium carbonate powder sample as raw material using the barium hydroxide octahydrate of high activity and hydrated titanium dioxide using low-temperature solid-phase method, and decentralized processing is carried out to obtain the nanoscale or submicron order high-purity barium titanate powder with good dispersion to barium carbonate powder sample by adding a certain amount of dispersant, this method decentralized processing process is simple, dispersion effect is apparent, dispersion stabilization is good, can effectively avoid powder reunite again and improve powder surface activity, there is very high production application value.
Description
Technical field
The invention belongs to the submicron order titaniums of inorganic functional powder body material technical field more particularly to a kind of good dispersion
Sour barium raw powder's production technology.
Background technology
Barium titanate is a kind of one of inorganic functional powder body material being widely used, because its with excellent ferroelectricity, piezoelectricity,
The performances such as low-dielectric loss and high-k, are mainly used in electronic material, ceramics, coating and machinery etc..Certain
Application field, the dispersibility and mobility of particle drastically influence the application performance of barium titanate.It is prepared in Super-fine Barium Titanate
Field, conventional solid method are difficult to reach sub-micron or nanoscale；Industrialized hydro-thermal method is although may be implemented sub-micron or receive
The preparation of scale particles, it is well known that particle is more tiny, specific surface energy is bigger, easier reunion, and method itself is existing
The cost problems such as liquid waste processing also affect the performance and market competition of barium carbonate powder.
Invention content
In order to solve the above technical problems, the object of the present invention is to provide a kind of submicron order barium titanate powders of good dispersion
Method prepared by body, the method are prepared by adding dispersant with good dispersion, stability, flowing using low-temperature solid-phase method
The barium carbonate powder of the advantages that property, good surface activity and small particle, the problems such as efficiently solving reunion, waste liquid and cost, in work
Industry produces and application aspect is valuable and potentiality.
The preparation method of the submicron order barium carbonate powder of a kind of good dispersion proposed by the present invention, by barium source and hydration
After titanium dioxide roasts at 50-1000 DEG C, dispersant processing is added in obtained barium carbonate powder.
Further, calcination temperature is 200-600 DEG C.
Further, roasting time 1-12h.
Further, roasting time 5-8h.
Further, barium source and the barium titanium molar ratio of hydrated titanium dioxide are 0.5-1.5：0.8-1.3.
Further, barium source include in barium hydroxide octahydrate, barium peroxide, barium acetate or barium nitrate any one or
It is a variety of.
Further, hydrated titanium dioxide include in α metatitanic acids, β metatitanic acids or titanium dioxide soaking object any one or it is more
Kind.
Further, the addition of dispersant is the 0.1%-5% of barium titanate powder weight.
Further, the mode of decentralized processing is that barium carbonate powder and dispersant are warming up to 25-400 DEG C, heat preservation
1-10h。
Further, dispersant includes polyethylene glycol, calcium stearate, dodecyl benzene sulfonic acid (sodium), magnesium stearate, 12
Any one or more in alkyl sulfonic acid (sodium), barium stearate, dodecyl sulphate (sodium), calcium laurate or stearic acid.
Further, the barium carbonate powder sample is cubic phase barium titanate or tetragonal-phase barium titanate.
It is another object of the present invention to propose a kind of submicron order titanium for the good dispersion being prepared by the above method
Sour barium powder.
It is another object of the present invention to propose the submicron order barium carbonate powder of above-mentioned good dispersion in electronic material, pottery
Application in ceramic material, coating and mechanical organ.
According to the above aspect of the present invention, the present invention has at least the following advantages：
1) barium carbonate powder prepared of the present invention has good dispersion and mobility, high-crystallinity, small particle and
The advantages of even subsphaeroidal or cube pattern, particle diameter distribution be narrow and submicrometer scale.
2) dispersant that the present invention selects derives from a wealth of sources, and of low cost, selected dispersant additive amount is few, dispersion effect
Obviously；Since selected dispersant decomposition temperature is low, therefore while sintering ceramics under the high temperature conditions, easily decomposes, will not be big in the product
Amount residual.
3) of the invention to be handled using dry dispersion, operating process is simple, and no waste liquid generates, and meets Green Chemistry and economy
Environmental protection concept, while the barium carbonate powder dispersion stabilization after decentralized processing is preferable.
Description of the drawings
Fig. 1 is the XRD diagram of the barium carbonate powder prepared described in embodiment 1.
Fig. 2 is the SEM figures of the barium carbonate powder prepared described in embodiment 1.
Fig. 3 is the XRD diagram of the barium carbonate powder prepared described in embodiment 2.
Fig. 4 is the SEM figures of the barium carbonate powder prepared described in embodiment 2.
Fig. 5 is the XRD diagram of the barium carbonate powder prepared described in embodiment 3.
Fig. 6 is the SEM figures of the barium carbonate powder prepared described in embodiment 3.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.
The person that is not specified actual conditions in embodiment, carries out according to conventional conditions or manufacturer's recommended conditions.Agents useful for same
Or production firm person is not specified in instrument, being can be with conventional products that are commercially available.
Embodiment 1
According to molar ratio 1：1 weighs barium hydroxide octahydrate and α metatitanic acids respectively, is placed in ball mill and is ground in 800r/min
It is taken out after 3h, is placed in Muffle furnace after roasting 5h at 600 DEG C and obtains barium carbonate powder sample.Take the above-mentioned 100g titaniums prepared
Sour barium powder sample, the calcium stearate dispersant that barium titanate powder weight 0.1% is added after mixing by the two are placed in 150
Barium carbonate powder is obtained after keeping the temperature 3h at DEG C.
Referring to Fig. 1, know through XRD characterization analysis, barium carbonate powder sample is tetragonal-phase barium titanate, and crystallinity is high.Referring to figure
2, know through SEM phenetic analysis, which has good homogeneity and dispersibility, and particle diameter distribution is narrow, and barium titanate is brilliant
Grain size is submicron order；By observing barium carbonate powder sample, there is good mobility, can keep steady well under normal conditions
Determine dispersion effect.
Embodiment 2
According to molar ratio 1：1 weighs barium hydroxide octahydrate and α metatitanic acids respectively, is placed in ball mill and is ground in 800r/min
It is taken out after 3h, is placed in Muffle furnace after roasting 8h at 200 DEG C and obtains barium carbonate powder sample.Take the above-mentioned 100g titaniums prepared
Sour barium powder sample, the polyethylene glycol dispersant that barium titanate powder weight 0.3% is added after mixing by the two are placed in 80
Barium carbonate powder sample is obtained after keeping the temperature 4h at DEG C.
Referring to Fig. 3, know through XRD characterization analysis, barium carbonate powder sample is cubic phase barium titanate, and crystallinity is high.Referring to figure
4, know through SEM phenetic analysis, which has good homogeneity and dispersibility, and particle diameter distribution is narrow, and barium titanate is brilliant
Grain size is submicron order；By observing barium carbonate powder sample, there is good mobility, can keep steady well under normal conditions
Determine dispersion effect.
Embodiment 3
According to molar ratio 1：1 weighs barium hydroxide octahydrate and α metatitanic acids respectively, is placed in ball mill and is ground in 800r/min
It is taken out after 3h, is placed in Muffle furnace after roasting 5h at 600 DEG C and obtains barium carbonate powder sample.Take the above-mentioned 100g titaniums prepared
Sour barium powder sample, the calcium laurate dispersant that barium titanate powder weight 0.8% is added after mixing by the two are placed in 200
Barium carbonate powder sample is obtained after keeping the temperature 4h at DEG C.
Referring to Fig. 5, know through XRD characterization analysis, barium carbonate powder sample is cubic phase barium titanate, and crystallinity is high.Referring to figure
6, know through SEM phenetic analysis, which has good homogeneity and dispersibility, and particle diameter distribution is narrow, and barium titanate is brilliant
Grain size is submicron order；By observing barium carbonate powder sample, there is good mobility, can keep steady well under normal conditions
Determine dispersion effect.
Comparative example 1
Data in table 1 are investigated, remaining processing step and parameter are same as Example 1, as a result such as table 1.
Table 1
Although the present invention has been described by way of example and in terms of the preferred embodiments, it is not limited to the present invention, any to be familiar with this skill
The people of art can do various change and modification, therefore the protection model of the present invention without departing from the spirit and scope of the present invention
Enclosing be subject to what claims were defined.
Claims (10)
1. a kind of preparation method of submicron order barium carbonate powder, it is characterised in that：By barium source and hydrated titanium dioxide in 50-
After being roasted at 1000 DEG C, dispersant progress decentralized processing is added in obtained barium carbonate powder.
2. the preparation method of submicron order barium carbonate powder according to claim 1, it is characterised in that：Roasting time is 1-
12h。
3. the preparation method of submicron order barium carbonate powder according to claim 1, it is characterised in that：Barium titanium molar ratio is
0.5-1.5：0.8-1.3.
4. the preparation method of submicron order barium carbonate powder according to claim 1, it is characterised in that：Barium source includes eight water
Close any one or more in barium hydroxide, barium peroxide, barium acetate or barium nitrate.
5. the preparation method of submicron order barium carbonate powder according to claim 1, it is characterised in that：Hydrated titanium dioxide
Including any one or more in α metatitanic acids, β metatitanic acids or titanium dioxide soaking object.
6. the preparation method of submicron order barium carbonate powder according to claim 1, it is characterised in that：The addition of dispersant
Amount is the 0.1%-5% of barium titanate powder weight.
7. the preparation method of submicron order barium carbonate powder according to claim 1, it is characterised in that：The side of decentralized processing
Formula is that barium carbonate powder and dispersant are warming up to 25-400 DEG C, keeps the temperature 1-10h.
8. the preparation method of submicron order barium carbonate powder according to claim 1, it is characterised in that：Dispersant includes poly-
Ethylene glycol, calcium stearate, dodecyl benzene sulfonic acid, neopelex, magnesium stearate, dodecyl sodium sulfonate, dodecane
In base sodium sulfonate, barium stearate, dodecyl sulphate, lauryl sodium sulfate, calcium laurate or stearic acid any one or
It is a variety of.
9. the submicron order barium carbonate powder that claim 1-8 any one of them methods are prepared.
10. the submicron order barium carbonate powder described in claim 9 is in electronic material, ceramic material, coating and mechanical organ
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3577487A (en) * | 1968-05-22 | 1971-05-04 | Grace W R & Co | Preparation of submicron sized alkaline earth titanate and zirconate powders |
| EP0318111B1 (en) * | 1987-11-25 | 1993-11-10 | Philips Patentverwaltung GmbH | Process for the preparation of barium titanate in powder form |
| CN1362385A (en) * | 2000-12-27 | 2002-08-07 | 株式会社村田制作所 | Barium titanate powder and preparation method thereof |
| CN1841588A (en) * | 2005-03-29 | 2006-10-04 | 三星电机株式会社 | Method for manufacturing dielectric ceramic powder, and multilayer ceramic capacitor |
| CN104828858A (en) * | 2015-04-14 | 2015-08-12 | 湖南先导电子陶瓷科技产业园发展有限公司 | Nanometer barium titanate powder preparation method based on ball milling |
| CN105271378A (en) * | 2015-09-29 | 2016-01-27 | 深圳市星源材质科技股份有限公司 | Preparation method of tetragonal barium titanate with high tetragonal rate |
-
2018
- 2018-05-16 CN CN201810465894.XA patent/CN108394932A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3577487A (en) * | 1968-05-22 | 1971-05-04 | Grace W R & Co | Preparation of submicron sized alkaline earth titanate and zirconate powders |
| EP0318111B1 (en) * | 1987-11-25 | 1993-11-10 | Philips Patentverwaltung GmbH | Process for the preparation of barium titanate in powder form |
| CN1362385A (en) * | 2000-12-27 | 2002-08-07 | 株式会社村田制作所 | Barium titanate powder and preparation method thereof |
| CN1841588A (en) * | 2005-03-29 | 2006-10-04 | 三星电机株式会社 | Method for manufacturing dielectric ceramic powder, and multilayer ceramic capacitor |
| CN104828858A (en) * | 2015-04-14 | 2015-08-12 | 湖南先导电子陶瓷科技产业园发展有限公司 | Nanometer barium titanate powder preparation method based on ball milling |
| CN105271378A (en) * | 2015-09-29 | 2016-01-27 | 深圳市星源材质科技股份有限公司 | Preparation method of tetragonal barium titanate with high tetragonal rate |
Non-Patent Citations (4)
| Title |
|---|
| O.ABE ET AL.: "Mechanochemically Assisted Preparation of BaTiO3 powder", 《MATERIALS SCIENCE FORUM》 * |
| 张圆圆: "低温固态反应制备纳米钙钛矿型物质及其机理研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 张超: "纳米材料PbTiO3、BaTiO3及BaxSr(1-x)TiO3的制备研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 王春杰等: "《纳米热障涂层材料》", 30 June 2017 * |
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Application publication date: 20180814 |