CN107673766A - A kind of structural ceramics high purity silicon nitride raw powder's production technology - Google Patents
A kind of structural ceramics high purity silicon nitride raw powder's production technology Download PDFInfo
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Abstract
The invention provides a kind of structural ceramics high purity silicon nitride raw powder's production technology, preparation process are as follows：（1）Pickling processes are carried out to raw material silica flour, and dried in vacuum or protective atmosphere.（2）Using the Si powder after above-mentioned processing as raw material, a certain proportion of diluent, activating agent are added.（3）The mixing and activation of above-mentioned raw materials are completed using high energy ball mill.Dried after ball milling under vacuum or protective atmosphere.（4）Powder after above-mentioned processing is put into nitriding furnace and nitrogenized in atmosphere.（5）Using the particle size and its distribution of high energy ball mill optimization beta-silicon nitride powder.Dried after ball milling under vacuum or protective atmosphere.The high purity silicon nitride silicon powder impurity content that the present invention announces is low, narrow particle size distribution, grain shape rule, has excellent sintering character, available for structural ceramics field.
Description
Technical field
The invention belongs to powder preparation field, specially a kind of structural ceramics high purity silicon nitride raw powder's production technology.
Background technology
Silicon nitride ceramic material is because with lightweight, hardness is high, rupture strength is big, thermal shock resistance is excellent, chemical stability
The features such as good, high temperature, high speed, strong corrosive medium working environment in show and greatly use space.At present, silicon nitride is made pottery
Porcelain has very wide application prospect in directions such as heat-resisting resistant to corrosion structural member, bearing, heat-conducting substrate, cutters.High-performance nitrogen
The preparation of SiClx ceramic material proposes higher requirement to the quality of beta-silicon nitride powder.
To obtain the excellent structural ceramics of comprehensive mechanical property, thin, close, even, pure is the important directions of development, and this is required
Beta-silicon nitride powder has higher purity to ensure the purity of product and the second phase is achieved effective control, it is desirable in powder contain compared with
Sintering activity of the pattern of high α phases, less particle diameter and rule to have obtained, it is desirable to powder with narrower size distribution with
Abnormal grain growth is avoided to cause intensity decreases.With silicon nitride ceramics using the extension in space, working environment it is increasingly harsh,
Higher requirement it is also proposed to the fracture toughness of silicon nitride ceramics.
The silicon nitride ceramics fracture toughness that current powder sintering goes out is poor, limits its application.Researcher is changing
Kind fracture toughness direction is explored, and main path has dis-persion toughening, fiber reinforced, transformation toughening, self toughening.
The content of the invention
Present invention is generally directed to the problem of structural ceramics comprehensive mechanical property difference, there is provided a kind of structural ceramics High Purity Nitrogen
SiClx raw powder's production technology.β phase particles in powder can be used as crystal seed in sintering process, be advantageous to the hair of β phase column crystals
Educate, by controlling its content to can control the content of column crystal.Sample purity made from the preparation method up to 99.9%, contain 2-
40% β phases, D50 are 0.5-1.0 μm, have the features such as narrow particle size distribution, grain shape rule, good dispersion, have after sintering
There is excellent comprehensive mechanical property.
The present invention provides a kind of structural ceramics high purity silicon nitride raw powder's production technology, comprises the following steps：
Step 1: the pickling processes of raw material Si powder
Pickling processes are carried out for the raw material silica flour of 200-500 mesh to granularity, to remove the SiO of metal impurities and surface2Film, improve
Si powder activity.Specific implementation method is：Si powder is cleaned with the HF or HCl of dilution with deionized water repeatedly, and in vacuum or guarantor
Dried in shield atmosphere.
Step 2: dispensing
Using the Si powder after above-mentioned processing as raw material, diluent, activating agent are added as following weight percent：
Si powder and activating agent are 60-90%, wherein, Si powder：Activating agent is 1:0.1-10；
（Si powder+activating agent）：Diluent is 10-40%.
Wherein, activating agent is porous silicon powder, amorphous silica powder or Si (NH2)2In one or more；Diluent is high α phases
Silicon nitride powder.
Step 3: ball milling
The mixing and activation of above-mentioned raw materials are completed using high energy ball mill.Specially：Grind the silicon nitride that Jie's ball is diameter 2-5 mm
Ceramics or zirconia ceramics ball, absolute ethyl alcohol is as ball-milling medium, ratio of grinding media to material 5:1-10:1, rotational speed of ball-mill 200-500 r/min,
Ball-milling Time 5-20 h.Dried after ball milling under vacuum or protective atmosphere.
Step 4: nitridation
Powder after above-mentioned processing is put into nitriding furnace and nitrogenized.Specially：After taking out vacuum twice, be passed through high-purity Ar gas or
Ar/H2Gaseous mixture, 1350-1400 DEG C is warming up to, vacuumized, be passed through N2、N2/H2Or N2/H2After/Ar, insulation 10-20 h, stop
Heating, in N2Room temperature is cooled in atmosphere.
Step 5: ball milling
Using the particle size and its distribution of high energy ball mill optimization beta-silicon nitride powder.Specially：It is diameter 2-5 mm's to grind Jie's ball
Silicon nitride ceramics or zirconia ceramics ball, ball-milling medium are absolute ethyl alcohol, and dispersant is 1% ammonium polyacrylate, ratio of grinding media to material 5:1-
10:1, rotational speed of ball-mill 200-500 r/min, Ball-milling Time 5-20 h.Dried after ball milling under vacuum or protective atmosphere.
Brief description of the drawings
Fig. 1 is the XRD spectrum of powder sample prepared by embodiment 1.
Fig. 2 is the scanning electron microscopic picture of powder sample prepared by embodiment 1.
Fig. 3 is the particle size distribution figure of powder sample prepared by embodiment 1.
Embodiment
The present invention is explained in detail below in conjunction with drawings and Examples.
Embodiment 1：
After the raw material silica flour that by purity be 99.99%, granularity is 200 mesh cleans 3 times with the HCl and deionized water of dilution, it is placed in true
In empty drying box, 10 h are dried at 85 DEG C.By the Si powder after above-mentioned processing：Porous silicon powder：The silicon nitride powder of high α phases（α phase contents
92%）Percentage by weight is 45 parts, 45 parts, 10 parts of the g of ratio dispensing 30.The mm of 300 g diameters 2 silicon nitride ceramic ball is added,
50 mL absolute ethyl alcohol, rotational speed of ball-mill are set to 300 r/min, the h of ball milling 20.In vacuum drying chamber, 10 are dried at 85 DEG C
After h, it is fitted into silicon nitride crucible.Silicon nitride crucible equipped with above-mentioned powder is put into nitriding furnace, after taking out vacuum twice, is passed through
High-purity Ar-H2Gaseous mixture（Ar：H2For 95:5）, 900 DEG C are warming up to, 1300 DEG C is warming up to after being incubated 0.5 h, is vacuumized, led to
N2-H2Gaseous mixture（N2：H2R is 95:5）Processing, after being incubated 2 h, 1350 DEG C are warming up to, adjusts N2：H2：Ar ratios are 90:5:5,
After being incubated 12 h, stop heating, in N2Room temperature is cooled in atmosphere.After sample taking-up, its grain is optimized using high energy ball mill
Degree and size distribution.Specially：30 g reactants are weighed, addition diameter 2 mm silicon nitride ceramic ball 300 g, 30 mL is anhydrous
Ethanol, 0.3 g ammonium polyacrylates, rotational speed of ball-mill is set as 500 r/min, the h of Ball-milling Time 20.In vacuum drying chamber, in 85
10 h are dried at DEG C.Slightly grinding obtains beta-silicon nitride powder in agate mortar afterwards.
The sample obtained to embodiment 1 carries out following test：By testing metals content impurity, it is pure to obtain beta-silicon nitride powder
Spend for 99.9%；Using XRD（X-ray Diffraction, X-ray diffraction）The phase structure of test sample（Fig. 1）；Using SEM
Test morphology microstructure（Fig. 2）；Particle size and its distribution is tested using laser particle analyzer（Fig. 3）.Fig. 1 is the XRD spectrum of sample, by
As a result understand, crystalline phase composition is α phases 94.9%, the silicon nitride of β phases 5.1%.By the SEM figures for sample（Fig. 2）Understand, contain in sample
There are a small amount of cylindrical particle, grain shape rule, soilless sticking phenomenon.From the figure 3, it may be seen that D50 is about 0.5 μm.
The sample and 2 wt%Al that embodiment 1 is obtained2O3-5 wt%Y2O3After being sufficiently mixed in high energy ball mill, it is placed in
In the graphite jig for scribbling BN, the N in hot pressing furnace2Sintered under atmosphere, hot pressing temperature is 1700 DEG C, the MPa of pressure 30, and insulation is protected
Press 40 min.Density measurement, bending strength test and fracture toughness test are carried out to the sample after sintering.After sintering, density can
Up to 3.25 g/cm3, intensity is up to 1001.5 MPa, fracture toughness up to 9.12 MPa/m1/2, there is excellent synthesis mechanical property
Energy.
Embodiment 2：
After the raw material silica flour that by purity be 99.9%, granularity is 300 mesh cleans 3 times with the HF and deionized water of dilution, tubular type is placed in
In stove, N210 h are dried at lower 120 DEG C of atmosphere.By the Si powder after above-mentioned processing：Si(NH2)2：The silicon nitride powder of high α phases（α phases contain
Amount 92%）Percentage by weight is 89 parts, 1 part, 10 parts of the g of ratio dispensing 60.Add the mm of 300 g diameters 3 zirconia ceramics
Ball, 60 mL absolute ethyl alcohol, rotational speed of ball-mill are set to 200 r/min, the h of ball milling 20.In tube furnace, N2At lower 120 DEG C of atmosphere
After drying 10 h, it is fitted into silicon nitride crucible.Silicon nitride crucible equipped with above-mentioned powder is put into nitriding furnace, takes out vacuum twice
Afterwards, high-purity Ar gas is passed through, is warming up to 1400 DEG C, is vacuumized, logical N2-H2-Ar（N2：H2：Ar is 95:5:0）Processing, insulation 2
After h, N is adjusted2：H2：Ar ratios, it is 90:5:5, after being incubated 18 h, stop heating, in N2Room temperature is cooled in atmosphere.Treat sample
After taking-up, its particle size and its distribution is optimized using high energy ball mill.Specially：Weigh 60 g reactants, addition diameter 2 mm
The g of zirconia ceramics ball 300,60 mL absolute ethyl alcohols, 0.6 g ammonium polyacrylates, set rotational speed of ball-mill as 500 r/min, ball
Consume time 15 h.In vacuum drying chamber, 10 h are dried at 85 DEG C.Slightly grinding obtains silicon nitride in agate mortar afterwards
Powder.
The sample obtained to embodiment 2 carries out test result：Sample purity is 99.2%；Crystalline phase composition for α phases 62.7%,
β phases 37.3%, containing a small amount of cylindrical particle, grain shape rule, soilless sticking phenomenon in sample, D50 is about 0.7 μm.
Embodiment 3：
After the raw material silica flour that by purity be 99.99%, granularity is 500 mesh cleans 3 times with the HF and deionized water of dilution, pipe is placed in
In formula stove, N210 h are dried at lower 120 DEG C of atmosphere.By the Si powder after above-mentioned processing：Amorphous silica powder：The silicon nitride powder of high α phases
Percentage by weight is 6 parts, 60 parts, 34 parts of the g of ratio dispensing 30.Add the mm of 300 g diameters 5 silicon nitride ceramic ball, 30 mL
Absolute ethyl alcohol, rotational speed of ball-mill is set to 500 r/min, the h of ball milling 10.In tube furnace, N210 h are dried at lower 120 DEG C of atmosphere
Afterwards, it is fitted into silicon nitride crucible.Silicon nitride crucible equipped with above-mentioned powder is put into nitriding furnace, after taking out vacuum twice, is passed through
High-purity Ar-H2Gaseous mixture（Ar：H2For 95:5）, 850 DEG C are warming up to, 1350 DEG C is warming up to after being incubated 0.5 h, is vacuumized, led to
N2-H2Gaseous mixture（N2：H2：Ar is 95:5）Processing, after being incubated 2 h, adjust N2：H2：Ar ratios, it is 90:5:5, after being incubated 13 h,
Stop heating, in N2Room temperature is cooled in atmosphere.After sample taking-up, its granularity and granularity point are optimized using high energy ball mill
Cloth.Specially：Weigh 30 g reactants, the addition diameter 2 mm g of silicon nitride ceramic ball 150,30 mL absolute ethyl alcohols, 0.3 g
Ammonium polyacrylate, rotational speed of ball-mill is set as 500 r/min, the h of Ball-milling Time 5.In vacuum drying chamber, 10 are dried at 85 DEG C
h.Slightly grinding obtains beta-silicon nitride powder in agate mortar afterwards.
The sample obtained to embodiment 3 carries out test result：Sample purity is 99.9%；Crystalline phase composition for α phases 98.1%,
β phases 1.9%, containing a small amount of cylindrical particle, grain shape rule, soilless sticking phenomenon in sample, D50 is about 1 μm.
Embodiment 4：
After the raw material silica flour that by purity be 99.99%, granularity is 200 mesh cleans 3 times with the HF and deionized water of dilution, pipe is placed in
In formula stove, N210 h are dried at lower 120 DEG C of atmosphere.By the Si powder after above-mentioned processing：Porous silicon：Si(NH2)2：The nitridation of high α phases
Silica flour percentage by weight is 47 parts, 12 parts, 12 parts, 30 parts of the g of ratio dispensing 30.Add the mm of 210 g diameters 2 zirconium oxide pottery
Porcelain ball, 30 mL absolute ethyl alcohol, rotational speed of ball-mill are set to 300 r/min, the h of ball milling 10.In tube furnace, N2Lower 120 DEG C of atmosphere
After 10 h of lower drying, it is fitted into silicon nitride crucible.Silicon nitride crucible equipped with above-mentioned powder is put into nitriding furnace, taken out true twice
After sky, high-purity Ar-H is passed through2Gaseous mixture（Ar：H2For 95:5）, 850 DEG C are warming up to, 1360 DEG C is warming up to after being incubated 0.5 h, carries out
Vacuumize, logical N2-H2Gaseous mixture（N2：H2：Ar is 95:5）Processing, after being incubated 2 h, adjust N2：H2：Ar ratios, it is 90:5:5, protect
After 13 h of temperature, stop heating, in N2Room temperature is cooled in atmosphere.After sample taking-up, its granularity is optimized using high energy ball mill
And size distribution.Specially：Weigh 30 g reactants, the addition diameter 2 mm anhydrous second of silicon nitride ceramic ball 200 g, 30 mL
Alcohol, 0.3 g ammonium polyacrylates, rotational speed of ball-mill is set as 500 r/min, the h of Ball-milling Time 15.In vacuum drying chamber, in 85 DEG C
10 h of lower drying.Slightly grinding obtains beta-silicon nitride powder in agate mortar afterwards.
The sample obtained to embodiment 4 carries out test result：Sample purity is 99.9%；Crystalline phase composition for α phases 95.3%,
β phases 4.7%, containing a small amount of cylindrical particle, grain shape rule, soilless sticking phenomenon in sample, D50 is about 0.86 μm.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of structural ceramics high purity silicon nitride raw powder's production technology, including the pickling processes of raw material, dispensing, ball milling mix
Activation, nitridation, ball milling optimization product 5 key steps of size distribution, the sample prepared is high-purity, high α phases, sintering character is excellent
Different beta-silicon nitride powder, it is characterised in that：
Step 1: raw material Si powder（Purity is not less than 99.9%）Pickling processes；
Step 2: dispensing：Using the Si powder after above-mentioned processing as raw material, a certain proportion of diluent, activating agent are added；
Step 3: ball milling：The mixing and activation of above-mentioned raw materials are completed using high energy ball mill, and is dried under vacuum or protective atmosphere
It is dry；
Step 4: nitridation：Powder after above-mentioned processing is put into nitriding furnace and nitrogenized in atmosphere；
Step 5: ball milling：Using the particle size and its distribution of high energy ball mill optimization beta-silicon nitride powder.
2. a kind of structural ceramics high purity silicon nitride raw powder's production technology according to claim 1, it is characterized in that：It is described
The step of one in, in pickling sour species for dilution HF or HCl.
3. a kind of structural ceramics high purity silicon nitride raw powder's production technology according to claim 1, it is characterized in that：It is described
The step of two in, activating agent is porous silicon powder, amorphous silica powder or Si (NH2)2In one or more.
4. a kind of structural ceramics high purity silicon nitride raw powder's production technology according to claim 3, it is characterized in that：Si powder
The 60-90% of raw material gross mass, Si powder are accounted for activating agent：Activating agent is 1:0.1-10.
5. a kind of structural ceramics high purity silicon nitride raw powder's production technology according to claim 1, it is characterized in that：It is described
The step of two in, diluent be purity higher than 99.9% high α phases or high β phases silicon nitride powder, principal crystalline phase content be higher than 92%,
（Si powder+activating agent）：Diluent is 10-40%.
6. a kind of structural ceramics high purity silicon nitride raw powder's production technology according to claim 1, it is characterized in that：It is described
The step of three in, silicon nitride ceramics or zirconia ceramics ball that mill Jie ball is diameter 2-5 mm, absolute ethyl alcohol as ball-milling medium,
Ratio of grinding media to material 5:1-10:1, rotational speed of ball-mill 200-500 r/min, Ball-milling Time 5-20 h.
7. a kind of structural ceramics high purity silicon nitride raw powder's production technology according to claim 1, it is characterized in that：It is described
The step of four in, the concrete operations of nitridation are that the silicon nitride crucible equipped with raw material is put into nitriding furnace, after taking out vacuum twice,
It is passed through high-purity Ar gas or Ar/H2Gaseous mixture, 1270-1400 DEG C is warming up to, vacuumized, be passed through N2、N2-H2Or N2-H2- Ar, insulation
After 10-40 h, stop heating, in N2Room temperature is cooled in atmosphere.
8. a kind of structural ceramics high purity silicon nitride raw powder's production technology according to claim 1, it is characterized in that：It is described
The step of five in, the design parameter of ball milling is：Grind the silicon nitride ceramics or zirconia ceramics ball that Jie's ball is diameter 2-5 mm, ball milling
Medium is absolute ethyl alcohol, ratio of grinding media to material 5:1-10:1, rotational speed of ball-mill 200-500 r/min, Ball-milling Time 5-40 h.
9. a kind of structural ceramics high purity silicon nitride raw powder's production technology according to claim 1, it is characterized in that：Prepare
β phase of the sample purity gone out up to 99.9%, containing 2-40%, there is the spies such as narrow particle size distribution, grain shape rule, good dispersion
Sign.
10. a kind of structural ceramics high purity silicon nitride raw powder's production technology according to claim 1, it is characterized in that：Should
For structural ceramics preparation field.
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Cited By (9)
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| CN109354503A (en) * | 2018-11-14 | 2019-02-19 | 江苏高越高新科技有限公司 | A kind of manufacture craft of silicon nitride ceramic ball |
| CN109970035A (en) * | 2019-04-04 | 2019-07-05 | 天津大学 | A kind of α-siliconnitride raw powder's production technology |
| CN109987943A (en) * | 2019-04-04 | 2019-07-09 | 天津大学 | A kind of preparation method of beta-silicon nitride powder |
| CN111253162A (en) * | 2019-02-22 | 2020-06-09 | 中国科学院上海硅酸盐研究所苏州研究院 | Method for preparing high-strength high-toughness high-thermal-conductivity silicon nitride ceramic |
| WO2020177465A1 (en) * | 2019-03-05 | 2020-09-10 | 青岛瓷兴新材料有限公司 | Silicon nitride, ceramic slurry and preparation method |
| WO2022011830A1 (en) * | 2020-07-14 | 2022-01-20 | 中材高新氮化物陶瓷有限公司 | Preparation method for silicon nitride powder |
| CN114716252A (en) * | 2022-04-27 | 2022-07-08 | 中国科学院上海硅酸盐研究所 | Preparation method of easy-to-sinter high-purity silicon nitride powder |
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