CN100358833C - Method for preparing ceramic material of zirconium phosphate - Google Patents
Method for preparing ceramic material of zirconium phosphate Download PDFInfo
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- CN100358833C CN100358833C CNB2006100188726A CN200610018872A CN100358833C CN 100358833 C CN100358833 C CN 100358833C CN B2006100188726 A CNB2006100188726 A CN B2006100188726A CN 200610018872 A CN200610018872 A CN 200610018872A CN 100358833 C CN100358833 C CN 100358833C
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Abstract
The present invention provides a method for preparing ceramic materials of zirconium phosphate. The method comprises the following steps: (1) zirconium orthophosphate powder is prepared, firstly, liquid phosphoric acid and the zirconia ceramic powder materials are directly mixed evenly, the weight proportioning of the liquid phosphoric acid to the zirconia ceramic powder materials is 2: 1, and then the heat treatment is carried out, so that the zirconium orthophosphate is generated by the thorough reaction of the zirconia and the phosphoric acid, and the zirconium phosphate is processed by calcining, ball milling, drying and sieving; (2) magnesia, alumina and silica are taken as addition agents and are evenly mixed with the zirconium orthophosphate powder; (3) the mixture is molded by dry pressing; (4) the molded mixture is processed by cold isostatic static pressure, and a base substrate is prepared; (5) the base substrate is sintered in normal atmosphere in 1100 to 1500 DEG C of air and preserves heat within 1 to 5 hours, and the zirconium phosphate ceramic materials are prepared. The present invention has the advantages of simple technology, good repeatability and lower cost. The prepared zirconium orthophosphate ceramic materials have the excellent capabilities of high density, higher mechanical (bending resistance) strength, low dielectric constant, low dielectric loss, etc.
Description
Technical field
The present invention relates to the stupalith field, particularly relate to a kind of preparation method of synthetic and pottery of zirconium phosphate powder.
Background technology
In recent years, the low bulk oxide ceramic material of resistant to elevated temperatures high strength, high stable becomes the research focus of new ceramic material, a kind of hi-tech new ceramic material that the zirconium phosphate pottery rises just on this basis.Because can prepare high strength, high temperature resistant, form compact and stable low bulk zirconium phosphate pottery by the zirconium phosphate powder, can widen the range of application of expansion ceramic material, so be subjected to the extensive concern of stupalith circle.The zirconium phosphate pottery is as a kind of excellent performance, the new ceramic material that has a extensive future, and its potential application can be distributed widely in chemical industry, electronics, military affairs etc.
Discover, the zirconium phosphate pottery also has lower specific inductivity and dielectric loss, thereby has expanded its range of application and Application Areas except having excellent comprehensive performances such as high strength, high temperature resistant, anti-thermal shock, low bulk, when the specific inductivity of material less than 10, dielectric loss is lower than 1 * 10
-2, can be used as electromagnetic wave transparent material and use.Therefore, the dielectric properties of research ceramic material of zirconium phosphate especially can prepare specific inductivity less than 10, and dielectric loss is lower than 1 * 10
-2The zirconium phosphate pottery, for it can find new application to be of great immediate significance in the electromagnetic wave transparent material field.
What generally adopt about the preparation of zirconium phosphate ceramic powder at present is chemical coprecipitation method, promptly utilizes zirconium oxychloride (ZrOCl
2) generate phosphoric acid one hydrogen zirconium (Zr (HPO with phosphatase reaction
4)
2) precipitation, after calcining, obtain zirconium phosphate (ZrP
2O
7) powder.The zirconium phosphate powder purity that this method prepares is higher, but the raw material of its use and technology cost height are unfavorable for producing in batches.The novel method that needs the higher zirconium phosphate powder of a kind of preparation purity with low cost, that be easy to realize of research, zirconium white (ZrO
2) be industrial raw material, cost is lower, and research zirconium white and phosphoric acid direct reaction synthesizing zirconium phosphate powder have stronger realistic meaning.
There are two big technological difficulties in the preparation of zirconium phosphate pottery: the one, and the pure phosphoric acid zircon ceramic is difficult for densification sintering, easily form vesicular structure, the pure phosphoric acid zirconium also is difficult to sintering at 1600 ℃, zirconium phosphate takes place to decompose slowly more than 1600 ℃, so the sintering temperature of zirconium phosphate pottery should be controlled at below 1600 ℃, reducing the sintering temperature of zirconium phosphate and forming fine and close structure mainly is to realize that by adding the metal oxide that can form phosphoric acid salt high-melting-point liquid phase the common sintering aid that is used for the sintering zirconium phosphate mainly contains: ZnO, MgO, Nb
2O
5, Ta
2O
5, TiO
2, Al
2O
3, SiO
2, zircon (ZrO
2-SiO
2) etc.The 2nd, the mechanical strength of zirconium phosphate pottery is lower, owing to individual die occurs grow up unusually between the high-temperature zone, the anisotropy of thermal expansion and cause producing tiny crack descends intensity significantly.Zirconium phosphate material is after 1400 ℃, and along with the rising of temperature, its crystal grain quickens to grow up, and particularly insulation is heated for a long time, and crystal grain is looked bigger, and the tiny crack of generation is more, though its thermal expansivity descends, also brings counter productive, causes strength degradation.As add TiO
2The zirconium phosphate material of 5wt.% was 1600 ℃ of sintering 30 minutes, and its folding strength has only 50MPa.
Consider above-mentioned two big difficult points and, when the zirconium phosphate pottery of sintering high-compactness, select MgO, Al for use for consideration to the dielectric material performance
2O
3, SiO
2Can considerable influence not arranged as sintering aid to the dielectric properties of burning till material.MgO is a kind of good fusing assistant, it and Al
2O
3Form the eutectic compound in lower temperature, can play fluxes promotes the effect of zirconium phosphate agglomerating; SiO
2Compound as additive and zirconium phosphate, it mainly contains two kinds of effects: the one, and SiO
2Has the excrescent effect of the zirconium phosphate crystal grain of inhibition; The 2nd, SiO
2Do not react with zirconium phosphate, and the quartzy material that belongs to low thermal coefficient of expansion, thermal expansivity is 2 * 10
-7℃
-1, better with the matching of zirconium phosphate.
By the new result of looking into of domestic and international patent and document is shown: also not about use phosphoric acid and zirconium white direct reaction synthesizing zirconium phosphate ceramic powder, and by selecting magnesium oxide, aluminum oxide and silicon oxide report for use as sintering aid densified sintering product ceramic material of zirconium phosphate.
Summary of the invention
Technical problem to be solved by this invention is: a kind of preparation method of ceramic material of zirconium phosphate is provided, and method is simple for this, can prepare to have excellent properties and lower-cost zirconium phosphate pottery, to meet the need of market.
The present invention solves its technical problem and adopts following technical scheme:
Comprise the preparation of zirconium phosphate powder and the sintering of zirconium phosphate pottery, specific as follows:
(1) preparation zirconium phosphate powder: elder generation is direct and zirconia ceramics powder uniform mixing with liquid phosphoric acid, and the weight proportion of the two is 2: 1, makes sample; Again sample is heat-treated, make zirconium white and phosphoric acid fully react the generation zirconium phosphate; Then to zirconium phosphate calcine, ball milling, drying, the processing of sieving, promptly get the zirconium phosphate powder.
(2) use any two or more mixture in magnesium oxide, aluminum oxide, the silicon oxide as complex sintering aids,, make mixture with zirconium phosphate powder uniform mixing.
(3) make mixture forming by the dry-pressing mode.
(4) forming mixture is carried out isostatic cool pressing and handle, make base substrate.
(5) base substrate is normal pressure-sintered in 1100～1500 ℃ of air, be incubated 1～5 hour, promptly get ceramic material of zirconium phosphate.
The present invention utilizes phosphoric acid and zirconium white complete reaction and generates a kind of like this synthesis mechanism of zirconium phosphate and prepares the higher zirconium phosphate ceramic powder of purity, simple for process, characteristics such as raw materials cost is low, favorable repeatability, synthetic powder purity is higher, particle diameter is less that this method has.Because the simple zirconium phosphate pottery that synthesizes is easy-sintering not, and zirconium phosphate crystal grain between the high-temperature zone is grown up unusually, owing to anisotropic thermal expansion causes producing tiny crack, intensity is descended significantly, so sintering zirconium phosphate pottery needs to add sintering aids and grain inhibitor.By adding MgO, Al
2O
3Fusing assistant, SiO
2Grain inhibitor is also allocated the proportioning of its component, can prepare have high-compactness, higher mechanics (bending resistance) intensity, and low-k (specific inductivity＜10) and dielectric loss (dielectric loss＜1 * 10
-2) ceramic material of zirconium phosphate.
In a word, technology of the present invention is simple, favorable repeatability, cost are low, and prepared ceramic material of zirconium phosphate has high-compactness, higher mechanics (bending resistance) intensity and excellent properties such as low-k and dielectric loss.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Fig. 2 is XRD (X-ray diffraction) figure of embodiment 1 product fracture.
Fig. 3 is the opticmicroscope figure of embodiment 1 product.
Fig. 4 is SEM (scanning electron microscope) figure of embodiment 2 product fractures.
Fig. 5 is the SEM figure of embodiment 3 product fractures.
Fig. 6 is the SEM figure of embodiment 4 product fractures.
Fig. 7 is the SEM figure of embodiment 5 product fractures.
Embodiment
The invention provides a kind of novel preparation method of ceramic material of zirconium phosphate, that is: elder generation synthesizes the zirconium phosphate powder under lower temperature, then to powder calcine, ball milling, drying, the processing of sieving, by adding magnesium oxide, aluminum oxide, silicon oxide sintering aid and allocating different proportionings, handle through isostatic cool pressing, high temperature sintering, make excellent performance and lower-cost ceramic material of zirconium phosphate.
Ceramic material of zirconium phosphate provided by the invention is to be undertaken by following step:
(1) preparation zirconium phosphate powder:
Elder generation is direct and zirconia ceramics powder uniform mixing with liquid phosphoric acid, and the weight proportion of the two is 2: 1, makes sample; Again sample is heat-treated, make zirconium white and phosphoric acid fully react the generation zirconium phosphate; Then to zirconium phosphate calcine, ball milling, drying, the processing of sieving, promptly get the zirconium phosphate powder.
In preparation zirconium phosphate powder process, can adopt weight concentration is 85% liquid phosphoric acid, and purity greater than 99.9%, particle diameter is less than the zirconia ceramics powder of 0.5 μ m.Under 250～500 ℃ and 1～5 hour condition of insulation, with sample thermal treatment.
(2) use magnesium oxide, aluminum oxide, silicon oxide as sintering aid,, make mixture with the synthetic zirconium phosphate powder uniform mixing that obtains.The doping of magnesium oxide, aluminum oxide is 0～5%, and the doping of silicon oxide is 0～2%.The purity of magnesium oxide, aluminum oxide and silicon oxide is greater than 99.9%, and particle diameter is less than 0.5 μ m.
(3) make mixture forming by the dry-pressing mode.Dry-pressing formed pressure is 5～20Mpa.
(4) forming mixture is carried out isostatic cool pressing and handle, make base substrate.The isostatic cool pressing processing pressure is 100～400Mpa.
(5) base substrate is normal pressure-sintered in 1100～1500 ℃ of air, temperature rise rate is 50～200 ℃/hour, is incubated 1～5 hour, can make specific inductivity less than 10 and dielectric loss less than 1 * 10
-2Ceramic material of zirconium phosphate.
The preparation of above-mentioned zirconium phosphate powder can be undertaken by following step:
(1) sample after the thermal treatment is calcined in 600～1000 ℃ of air.
(2) during the sample after will calcining is packed agate jar into, be that solvent, agate ball are grinding medium with the dehydrated alcohol, ball milling 12～48 hours.
(3), cross 100 mesh sieves with behind the powder drying behind the ball milling.
The invention will be further described below in conjunction with embodiment and accompanying drawing.
The invention provides a kind of synthetic, processing and zirconium phosphate ceramic sintering process of novel zirconium phosphate powder, its technical process is as shown in Figure 1: comprise the operation that adopts phosphoric acid and the high-purity fine powder direct reaction of zirconium white synthesizing zirconium phosphate powder, the mixing of the calcining of zirconium phosphate powder, ball milling, drying, the operation handled of sieving and zirconium phosphate powder and sintering aid, dry-pressing formed, isostatic cool pressing processing and normal pressure-sintered operation.
Embodiment 1:
(1) with weight concentration is 85% phosphoric acid (H
3PO
4) with the meta particle diameter be the zirconium white (ZrO of 0.2 μ m
2) fine powder (purity＞99.9%) is 2: 1 uniform mixing according to weight ratio;
(2) compound is heat-treated at 350 ℃, and be incubated 2 hours, zirconium white and phosphoric acid are fully reacted, generate zirconium phosphate (ZrP
2O
7);
(3) product was calcined 1 hour at 700 ℃, powder after the calcining is packed in the agate jar, is solvent (grinding medium is an agate ball) ball milling 24 hours with the dehydrated alcohol, utilizes the oven for drying powder, cross 100 mesh sieves, obtain the higher zirconium phosphate ceramic powder of purity.
Analytical test shows that (see Fig. 2, Fig. 3): zirconium white and phosphatase reaction can generate zirconium phosphate one-component crystalline phase fully at 250 ℃, and the thing of product is ZrP mutually
2O
7, do not find remaining zirconium white (ZrO
2) the thing phase.Through 1000 ℃ of calcinings, the thing of product still is ZrP mutually
2O
7, do not undergo phase transition.Illustrate that adopting phosphoric acid and zirconium white direct reaction to prepare zirconium phosphate has higher purity, the zirconium phosphate powder has stability preferably.The opticmicroscope picture of synthetic zirconium phosphate powder shows that the particle diameter of powder is less, and particle diameter is about 1 μ m.
Embodiment 2:
(1) (granularity is 0.2 μ m with synthetic zirconium phosphate powder and magnesium oxide in the embodiment 1, purity is 99.9%), (granularity is 0.2 μ m to aluminum oxide, purity is 99.9%), the high-purity fine powder of silicon oxide (granularity is 0.5 μ m, and purity is 99.9%) is 90: 4: 4 according to weight ratio: 2 uniform mixing;
(2) dry-pressing formed by 10MPa;
(3) handle by the 400MPa isostatic cool pressing;
(4) carry out normal pressure-sinteredly at 1200 ℃, temperature rise rate is 100 ℃/h and is incubated 5 hours;
(5) furnace cooling.Can obtain density is 95.8%, and bending strength is 102MPa, and specific inductivity is 7.5, and dielectric loss is 4.0 * 10
-3The ceramic material of zirconium phosphate of (frequency is 1GHz).
Analytical test shows (see figure 4): SEM figure shows that the zirconium phosphate ceramic dense degree for preparing is higher, still has a small amount of pore, and zirconium phosphate crystallization situation is better, can observe cubic crystal, does not find growing up unusually of crystal grain; At the section of material, transgranular fracture has mainly taken place in crystal grain, also has some along brilliant crack conditions, and this explanation agglomerating zirconium phosphate ceramic grain-boundary place has higher intensity, and this material has higher bending strength.
Embodiment 3:
(1) (granularity is 0.2 μ m with synthetic zirconium phosphate powder and magnesium oxide in the embodiment 1, purity is 99.9%), (granularity is 0.2 μ m to aluminum oxide, purity is 99.9%), the high-purity fine powder of silicon oxide (granularity is 0.5 μ m, and purity is 99.9%) is 92: 4: 4 according to weight ratio: 0 uniform mixing;
(2) dry-pressing formed by 20MPa;
(3) handle by the 200MPa isostatic cool pressing;
(4) carry out normal pressure-sinteredly at 1300 ℃, temperature rise rate is 200 ℃/h and is incubated 5 hours;
(5) furnace cooling.Can obtain density is 98.5%, and bending strength is 131MPa, and specific inductivity is 8.8, and dielectric loss is 7.5 * 10
-3The ceramic material of zirconium phosphate of (frequency is 1GHz).
Analytical test shows (see figure 5): SEM figure shows the zirconium phosphate ceramic dense degree height for preparing, and zirconium phosphate crystallization situation is better, does not find growing up unusually of crystal grain; At the section of material, transgranular fracture has taken place in crystal grain, and this explanation agglomerating zirconium phosphate ceramic grain-boundary place has higher intensity, and this material has higher bending strength.
Embodiment 4:
(1) (granularity is 0.2 μ m with synthetic zirconium phosphate powder and magnesium oxide in the embodiment 1, purity is 99.9%), (granularity is 0.2 μ m to aluminum oxide, purity is 99.9%), the high-purity fine powder of silicon oxide (granularity is 0.5 μ m, and purity is 99.9%) is 95: 5: 0 according to weight ratio: 0 uniform mixing;
(2) dry-pressing formed by 10MPa;
(3) handle by the 200MPa isostatic cool pressing;
(4) carry out normal pressure-sinteredly at 1400 ℃, temperature rise rate is 100 ℃/h and is incubated 5 hours;
(5) furnace cooling.Can obtain density is 99.0%, and bending strength is 125MPa, and specific inductivity is 8.2, and dielectric loss is 6.0 * 10
-3The ceramic material of zirconium phosphate of (frequency is 1GHz).
Analytical test shows (see figure 6): SEM figure shows that the zirconium phosphate ceramic dense degree for preparing is very high, and zirconium phosphate crystallization situation is better, and grain growth is apparent in view, does not find growing up unusually of individual die; At the section of material, transgranular fracture has taken place in crystal grain, and this explanation agglomerating zirconium phosphate ceramic grain-boundary place has high intensity, and this material has higher bending strength.
Embodiment 5:
(1) (granularity is 0.2 μ m with synthetic zirconium phosphate powder and magnesium oxide in the embodiment 1, purity is 99.9%), (granularity is 0.2 μ m to aluminum oxide, purity is 99.9%), the high-purity fine powder of silicon oxide (granularity is 0.5 μ m, and purity is 99.9%) is 94: 4: 0 according to weight ratio: 2 uniform mixing;
(2) dry-pressing formed by 10MPa;
(3) handle by the 200MPa isostatic cool pressing;
(4) carry out normal pressure-sinteredly at 1500 ℃, temperature rise rate is 200 ℃/h and is incubated 2 hours;
(5) furnace cooling.Can obtain density is 99.5%, and bending strength is 132MPa, and specific inductivity is 8.5, and dielectric loss is 7.0 * 10
-3The ceramic material of zirconium phosphate of (frequency is 1GHz).
Analytical test shows (see figure 7): SEM figure shows that the zirconium phosphate ceramic dense degree for preparing is very high, and zirconium phosphate crystallization situation is better, and grain growth is apparent in view, does not find growing up unusually of individual die; At the section of material, transgranular fracture has taken place in crystal grain, and this explanation agglomerating zirconium phosphate ceramic grain-boundary place has high intensity, and this material has higher bending strength.
The foregoing description is not a limitation of the present invention, and it can be used as further understands the present invention.
Claims (10)
1. the preparation method of a ceramic material of zirconium phosphate comprises the preparation of zirconium phosphate powder and the sintering of zirconium phosphate pottery, it is characterized in that being undertaken by following step:
(1) preparation zirconium phosphate powder:
Elder generation is direct and zirconia ceramics powder uniform mixing with liquid phosphoric acid, and the weight proportion of the two is 2: 1, makes sample,
Again sample is heat-treated, makes zirconium white and phosphoric acid fully react the generation zirconium phosphate,
Then to zirconium phosphate calcine, ball milling, drying, the processing of sieving, promptly get the zirconium phosphate powder,
(2) any two or more mixture in use magnesium oxide, aluminum oxide, the silicon oxide with zirconium phosphate powder uniform mixing, makes mixture as complex sintering aids,
(3) make mixture forming by the dry-pressing mode,
(4) forming mixture is carried out isostatic cool pressing and handles, make base substrate,
(5) base substrate is normal pressure-sintered in 1100～1500 ℃ of air, be incubated 1～5 hour, promptly get ceramic material of zirconium phosphate.
2. the preparation method of ceramic material of zirconium phosphate according to claim 1, it is characterized in that adopting weight concentration is 85% liquid phosphoric acid.
3. the preparation method of ceramic material of zirconium phosphate according to claim 1 is characterized in that: adopt purity greater than 99.9%, particle diameter is less than the zirconia ceramics powder of 0.5 μ m.
4. the preparation method of ceramic material of zirconium phosphate according to claim 1 is characterized in that: sample was heat-treated under the condition with insulation at 250～500 ℃ in 1～5 hour.
5. the preparation method of ceramic material of zirconium phosphate according to claim 1 is characterized in that: by following step zirconium phosphate is made the zirconium phosphate powder,
(1) sample after the thermal treatment is calcined in air,
(2) during the sample after will calcining is packed agate jar into, be that solvent, agate ball are grinding medium with the dehydrated alcohol, ball milling 12～48 hours,
(3), cross 100 mesh sieves with behind the powder drying behind the ball milling.
6. the preparation method of ceramic material of zirconium phosphate according to claim 5, it is characterized in that: calcining temperature is 600～1000 ℃.
7. the preparation method of ceramic material of zirconium phosphate according to claim 1, it is characterized in that: the doping of magnesium oxide, aluminum oxide is respectively 0～5%, and the doping of silicon oxide is 0～2%.
8. the preparation method of ceramic material of zirconium phosphate according to claim 7, it is characterized in that: the purity of magnesium oxide, aluminum oxide and silicon oxide is greater than 99.9%, and particle diameter is less than 0.5 μ m.
9. the preparation method of ceramic material of zirconium phosphate according to claim 1, it is characterized in that: dry-pressing formed pressure is 5～20MPa, and the isostatic cool pressing processing pressure is 100～400Mpa, and normal pressure-sintered temperature rise rate is 50～200 ℃/hour.
10. the preparation method of ceramic material of zirconium phosphate according to claim 1, it is characterized in that: the specific inductivity of zirconium phosphate pottery is less than 10, and dielectric loss is less than 1 * 10
-2
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| CN104876612A (en) * | 2015-04-13 | 2015-09-02 | 安徽省含山瓷业股份有限公司 | High-strength carbon fiber reinforced zirconium phosphate ceramic matrix composite and preparation method thereof |
| JP6190023B1 (en) * | 2015-10-07 | 2017-08-30 | 日本化学工業株式会社 | Method for producing zirconium tungstate phosphate |
| CN110937889B (en) * | 2019-12-10 | 2022-03-04 | 武汉科技大学 | Zirconium phosphate ceramic material and preparation method thereof |
| CN114751731B (en) * | 2022-04-11 | 2023-07-21 | 武汉科技大学 | Zirconium pyrophosphate composite porous ceramic material based on foaming method and preparation method thereof |
| CN115322490A (en) * | 2022-08-23 | 2022-11-11 | 广东圆融新材料有限公司 | Extrusion-grade low-dielectric-constant polypropylene material and preparation method thereof |
| CN115417669A (en) * | 2022-09-30 | 2022-12-02 | 武汉科技大学 | High silica glass fiber reinforced zirconium pyrophosphate-based composite material and preparation method thereof |
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| US20020132720A1 (en) * | 2000-09-27 | 2002-09-19 | Cutler Willard A. | Refractory NZP-type structures and method of making and using same |
| CN1597611A (en) * | 2004-07-21 | 2005-03-23 | 昆明理工大学 | Phosphate ceramicd material Ca1, Ba, Zr4, P6, O24 with zero expansion chnracteristicc and its preparation method |
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|---|---|---|---|---|
| US20020132720A1 (en) * | 2000-09-27 | 2002-09-19 | Cutler Willard A. | Refractory NZP-type structures and method of making and using same |
| CN1597611A (en) * | 2004-07-21 | 2005-03-23 | 昆明理工大学 | Phosphate ceramicd material Ca1, Ba, Zr4, P6, O24 with zero expansion chnracteristicc and its preparation method |
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