CN104694017A - Preparation method of polishing powder for polishing of silicon nitride ceramics - Google Patents
Preparation method of polishing powder for polishing of silicon nitride ceramics Download PDFInfo
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- CN104694017A CN104694017A CN201510126391.6A CN201510126391A CN104694017A CN 104694017 A CN104694017 A CN 104694017A CN 201510126391 A CN201510126391 A CN 201510126391A CN 104694017 A CN104694017 A CN 104694017A
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- silicon nitride
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
Abstract
The invention discloses a preparation method of polishing powder for polishing of silicon nitride ceramics. The preparation method is characterized by comprising the following steps that 8-11% of cerium chloride, 28-38% of chromium trioxide and 2-5% of sodium dedecyl benzene sulfonate by mass are added to be dissolved in water in a reactor according to the weight percentage concentration, then 10-20% of aluminum oxide and 32-45% of boron nitride are added and stirred to be in a size state, then 3-8% of oxalic acid is dissolved in water and then added, the sum of all the components is 100%, water is not included into the components, the mixture is stirred under normal pressure, is heated to 85 DEG C, and reacts for 18-24 hours, cerium chloride generates cerous oxalate with even particles, solid and liquid are separated, the cerous oxalate is roasted for 5-8 hours at 1100-1150 DEG C, and polishing powder for silicon nitride ceramics is obtained after cooling and fluid energy milling. The polishing powder has the advantages of being high in polishing hardness and good in powder polishing effect, high in glossiness, free of scratches, high in flatness and small in usage amount.
Description
Technical field
What the present invention relates to is a kind of preparing technical field of polishing powder, particularly a kind of silicon nitride ceramics polishing powder preparation technology and in silicon nitride ceramics polishing.
Background technology
Silicon nitride is the compound synthesized under artificial condition.Though just directly synthesized silicon nitride before more than 140 years, the nitride at that time as just a kind of stable " infusibility " has been stayed in the memory of people.After World War II, developing rapidly, in the urgent need to high temperature resistant, high rigidity, high strength, erosion-resisting material of science and technology.Through long-term effort, until nineteen fifty-five silicon nitride be just taken seriously, middle nineteen seventies has just really obtained high quality, low cost, has the silicon nitride ceramics of extensive important use.
The intensity of silicon nitride is very high, especially hot pressed silicon nitride (HPSN), is one of the hardest in the world material.It is extremely high temperature resistant, and intensity can be maintained to the high temperature of 1200 DEG C always and not decline, and can not be melt into melt body after being heated, until 1900 DEG C just can be decomposed, and have surprising resistance to chemical corrosion, the mineral acid that ability is nearly all and less than 30% caustic soda soln, also ability a lot of organic acid corrosion; Again a kind of high-performance electric insulating material simultaneously.
Silicon nitride is a kind of important structural ceramic material.It is a kind of superhard material, and itself has oilness, and wear-resistant, is atomic crystal; Anti-oxidant during high temperature.And it can also resist thermal shock, be heated to more than 1000 DEG C in atmosphere, quick refrigeration sharply heats again, also can not be cracked.Have so excellent characteristic just because of silicon nitride ceramics, people usually utilize it to manufacture the mechanical components such as bearing, blade of gas turbine, mechanical seal ring, permanent mold.If manufacture the heating surface of engine parts with silicon nitride ceramics that is high temperature resistant and that do not readily conduct heat, not only can improve diesel engine quality, fuel saving, and can thermo-efficiency be improved.Therefore its polishing process in ganoid silicon nitride ceramics process is manufactured very important.
Silicon nitride ceramics production technique comprises: shaping → sintering → corase grind → polishing → polishing.The quality of silicon nitride ceramics polishing process quality directly affects the quality of its product, and polishing process is very important in silicon nitride ceramics production process thus, and polishing powder used in polishing process directly affects the quality of finish of silicon nitride ceramics.
The polishing of silicon nitride ceramics is an extremely complicated mechanochemical process.In this process, except mechanical effect, also have silicon nitride ceramics component, chemical action between polishing powder composition and polished die composition.Therefore, in polishing powder system, the change of chemical constitution, will cause the adhesive power between polished die and silicon nitride ceramics to change, and also causes changing in work area temperature, polishing powder concentration, finally affects polishing efficiency.Therefore, the chemical constitution of polishing powder is most important to silicon nitride ceramics polishing effect.Silicon nitride ceramics hardness is comparatively spent high, and crystal grain is tiny, even.Highly polished after polished finish, so need polishing powder to have very high hardness when processing silicon nitride ceramics, soft fine and smooth again.
With regard to polishing powder, different polishing powders has different polishing abilities.Polishing powder is made up of components such as cerium oxide, aluminum oxide, silicon oxide, ferric oxide, zirconium white, chromic oxide, stannic oxide usually, and the hardness of different materials is different, and the chemical property in water is also different, and therefore use occasion is different.The Mohs' hardness of aluminum oxide and chromic oxide is 9, and cerium oxide and zirconium white are 7, and ferric oxide is lower.In silicon carbide ceramics polishing process, add polishing powder, present people use chromium sesquioxide powder mostly, namely adopt single abrasive material and single polishing powder to carry out polishing, but the polishing of this single polishing powder to silicon nitride ceramics does not reach excellent polishing effect.May be that single polishing powder is in polishing friction process.Between the powder of polishing powder, mobility or soft durometer can not be complementary.Several oxide compound is composite can overcome above-mentioned deficiency, a kind of composite polishing powder of polishing of optical element and preparation method and glossing is disclosed in Chinese patent application CN101362925B, be have the chromium sesquioxide of 0.5 part ~ 3 parts and the aluminium sesquioxide of 1.0 parts to form, but the wear resistance of this compound polishing powder does not reach the polishing requirement of silicon nitride ceramics.
Boron nitride is corrosion-resistant, and electrical insulating property is fine, and usually obtained boron nitride is graphite structure, is commonly called as white graphite.Another kind is diamond-type, and graphite to change adamantine principle into similar, graphite mould boron nitride can change Buddha's warrior attendant type boron nitride under high temperature (1800 DEG C), high pressure (8000Mpa) [5 ~ 18GPa].Be the superhard material of novel fire resistant, Mohs' hardness is more than 10, and its epigranular, hardness are high, self-sharpening is strong, and cutting power is comparatively strong, and stable chemical nature, thermal conductivity is good.Boron nitride and rare earth oxide, chromic oxide are prepared a kind of polishing powder for silicon nitride ceramics polishing by the application, this polishing powder has that hardness is high, good fluidity and thermal conductivity is good, soft durometer can not be complementary etc. advantage.
Summary of the invention
The one that is to provide order of the present invention can reduce polishing cut, improve polishing powder gouge hardness, improves preparation method and the technique of the polishing powder of silicon nitride ceramics smooth finish;
Object of the present invention is achieved through the following technical solutions.
A kind of preparation method of silicon nitride ceramics polishing powder, be characterised in that the method has following processing step: in the reactor, add the Cerium II Chloride of 8% ~ 11% by mass percentage, the chromium trioxide of 28% ~ 38%, 2% ~ 5% Sodium dodecylbenzene sulfonate is dissolved in the water, add the aluminium sesquioxide of 10% ~ 20% again, the boron nitride of 32% ~ 45%, stir in slurries, again 3% ~ 8% dissolving oxalic acid is added after water, each component sum is absolutely, water is not counted in component, under normal pressure, stir, add heat 85 DEG C, reaction 18 ~ 24h, Cerium II Chloride is made to generate evengranular Sedemesis, solid-liquid separation, at 1100 DEG C ~ 1150 DEG C roasting 5 ~ 8h, after cooling, through comminution by gas stream, obtain silicon nitride ceramics polishing powder, the particle diameter of the silicon nitride ceramics polishing powder obtained is in the scope of 0.2 ~ 2.0 μm.
In a kind of preparation method of silicon nitride ceramics polishing powder, described boron nitride is Buddha's warrior attendant type boron nitride.
In a kind of preparation method of silicon nitride ceramics polishing powder, described Cerium II Chloride is anhydrous cerium chloride.
In a kind of preparation method of silicon nitride ceramics polishing powder, described aluminium sesquioxide, boron nitride, its particle diameter is 0.2 ~ 1.5 μm of scope.
In a kind of preparation method of silicon nitride ceramics polishing powder, described chloric acid cerium: the optimum molar ratio of oxalic acid will between 1:1.5.
In a kind of preparation method of silicon nitride ceramics polishing powder, the effect of ammonium oxalate Cerium II Chloride oxalic cerium is precipitated be attached to the surface of solid phase, excessive ammonium oxalate by thermal degradation on product without impact.
Particle size test method of the present invention is the granularity equivalent diameter size adopting laser particle analyzer to record.
The silicon nitride ceramics polishing powder method that the present invention obtains: namely may be used for wet throwing and also can be used for dry throwing, every square metre of consumption is 15 ~ 20g.
Compared with the prior art, tool has the following advantages and beneficial effect in the present invention:
(1) the present invention obtains silicon nitride ceramics polishing powder, in preparation process, adopts and adds boron nitride component, the polishing gouge hardness of polishing powder is significantly improved, may be used for the polishing of various high hardness silicon nitride ceramics.
(2) the present invention obtains silicon nitride ceramics polishing powder, in preparation process, adding ammonium oxalate is precipitation agent, ammonium oxalate is decomposing oxalic acid root in heat-processed, making the concentration of system oxalate consistent is precipitation from homogeneous solution (PFHS) system with Cerium II Chloride oxalic cerium, and so formation Sedemesis particle is tiny and even.After oversintering, the particle fine uniform of chromium trioxide, Sedemesis generation cerium oxide, chromium sesquioxide is distributed in aluminium sesquioxide, boron nitride on the surface, there is meso-position radius grain little, the feature that particle size distribution is narrow, between the powder simultaneously making polishing powder mobility or soft durometer complementary, reach better polishing effect.
(3) the present invention obtains silicon nitride ceramics polishing powder, and preparation technology is simple, and condition is easy to control, and production cost is low, is easy to suitability for industrialized production.
Embodiment
Embodiment 1
A kind of preparation method of silicon nitride ceramics polishing powder, in the reactor, add the Cerium II Chloride of 9g respectively, the chromium trioxide of 32g, 3g Sodium dodecylbenzene sulfonate is dissolved in the water, add the aluminium sesquioxide of 15g again, the boron nitride of 36g, stir in slurries, again 5g dissolving oxalic acid is added after water, water is not counted in component, under normal pressure, stir, add heat 85 DEG C, reaction 21h, Cerium II Chloride is made to generate evengranular Sedemesis, solid-liquid separation, at 1100 DEG C of roasting 6h, after cooling, through comminution by gas stream, obtain silicon nitride ceramics polishing powder, the particle diameter of the silicon nitride ceramics polishing powder obtained is in the scope of 0.2 ~ 2.0 μm.
Embodiment 2
A kind of preparation method of silicon nitride ceramics polishing powder, in the reactor, add the Cerium II Chloride of 8g respectively, the chromium trioxide of 36g, 2g Sodium dodecylbenzene sulfonate is dissolved in the water, add the aluminium sesquioxide of 12g again, the boron nitride of 38g, stir in slurries, again 4g dissolving oxalic acid is added after water, water is not counted in component, under normal pressure, stir, add heat 85 DEG C, reaction 18h, Cerium II Chloride is made to generate evengranular Sedemesis, solid-liquid separation, at 1150 DEG C of roasting 7h, after cooling, through comminution by gas stream, obtain silicon nitride ceramics polishing powder, the particle diameter of the silicon nitride ceramics polishing powder obtained is in the scope of 0.2 ~ 2.0 μm.
Embodiment 3
A kind of preparation method of silicon nitride ceramics polishing powder, in the reactor, add the Cerium II Chloride of 11g respectively, the chromium trioxide of 28g, 4g Sodium dodecylbenzene sulfonate is dissolved in the water, add the aluminium sesquioxide of 10g again, the boron nitride of 41g, stir in slurries, again 6g dissolving oxalic acid is added after water, water is not counted in component, under normal pressure, stir, add heat 85 DEG C, reaction 22h, Cerium II Chloride is made to generate evengranular Sedemesis, solid-liquid separation, at 1130 DEG C of roasting 8h, after cooling, through comminution by gas stream, obtain silicon nitride ceramics polishing powder, the particle diameter of the silicon nitride ceramics polishing powder obtained is in the scope of 0.2 ~ 2.0 μm.
Embodiment 4
A kind of preparation method of silicon nitride ceramics polishing powder, in the reactor, add the Cerium II Chloride of 10g respectively, the chromium trioxide of 30g, 5g Sodium dodecylbenzene sulfonate is dissolved in the water, add the aluminium sesquioxide of 18g again, the boron nitride of 32g, stir in slurries, again 5g dissolving oxalic acid is added after water, water is not counted in component, under normal pressure, stir, add heat 85 DEG C, reaction 23h, Cerium II Chloride is made to generate evengranular Sedemesis, solid-liquid separation, at 1140 DEG C of roasting 5h, after cooling, through comminution by gas stream, obtain silicon nitride ceramics polishing powder, the particle diameter of the silicon nitride ceramics polishing powder obtained is in the scope of 0.2 ~ 2.0 μm.
Embodiment 5
A kind of preparation method of silicon nitride ceramics polishing powder, in the reactor, add the Cerium II Chloride of 9g respectively, the chromium trioxide of 38g, 2g Sodium dodecylbenzene sulfonate is dissolved in the water, add the aluminium sesquioxide of 13g again, the boron nitride of 34g, stir in slurries, again 4g dissolving oxalic acid is added after water, water is not counted in component, under normal pressure, stir, add heat 85 DEG C, reaction 24h, Cerium II Chloride is made to generate evengranular Sedemesis, solid-liquid separation, at 1130 DEG C of roasting 6.5h, after cooling, through comminution by gas stream, obtain silicon nitride ceramics polishing powder, the particle diameter of the silicon nitride ceramics polishing powder obtained is in the scope of 0.2 ~ 2.0 μm.
Embodiment 6
A kind of preparation method of silicon nitride ceramics polishing powder, in the reactor, add the Cerium II Chloride of 8g respectively, the chromium trioxide of 34g, 3g Sodium dodecylbenzene sulfonate is dissolved in the water, add the aluminium sesquioxide of 10g again, the boron nitride of 42g, stir in slurries, again 3g dissolving oxalic acid is added after water, water is not counted in component, under normal pressure, stir, add heat 85 DEG C, reaction 19h, Cerium II Chloride is made to generate evengranular Sedemesis, solid-liquid separation, at 1150 DEG C of roasting 7.5h, after cooling, through comminution by gas stream, obtain silicon nitride ceramics polishing powder, the particle diameter of the silicon nitride ceramics polishing powder obtained is in the scope of 0.2 ~ 2.0 μm.
Using method: namely may be used for wet throwing and also can be used for dry throwing, by polishing powder and water furnishing starchiness during wet throwing, wet throwing is selected in suggestion, because dry polishing powder dirt can pollute.
The present invention obtains silicon nitride ceramics polishing powder, and powder polishing effect is good, glossiness, and can reach more than 99 degree, no marking, planeness is high, and the consumption of powder is few.
Claims (5)
1. the preparation method of a silicon nitride ceramics polishing powder, be characterised in that the method has following processing step: in the reactor, add the Cerium II Chloride of 8% ~ 11% by mass percentage, the chromium trioxide of 28% ~ 38%, 2% ~ 5% Sodium dodecylbenzene sulfonate is dissolved in the water, add the aluminium sesquioxide of 10% ~ 20% again, the boron nitride of 32% ~ 45%, stir in slurries, again 3% ~ 8% dissolving oxalic acid is added after water, each component sum is absolutely, water is not counted in component, under normal pressure, stir, add heat 85 DEG C, reaction 18 ~ 24h, Cerium II Chloride is made to generate evengranular Sedemesis, solid-liquid separation, at 1100 DEG C ~ 1150 DEG C roasting 5 ~ 8h, after cooling, through comminution by gas stream, obtain silicon nitride ceramics polishing powder, the particle diameter of the silicon nitride ceramics polishing powder obtained is in the scope of 0.2 ~ 2.0 μm.
2., in the preparation method of a kind of silicon nitride ceramics polishing powder according to claim 1, it is characterized in that, described boron nitride is Buddha's warrior attendant type boron nitride.
3., in the preparation method of a kind of silicon nitride ceramics polishing powder according to claim 1, it is characterized in that, described Cerium II Chloride is anhydrous cerium chloride.
4., in the preparation method of a kind of silicon nitride ceramics polishing powder according to claim 1, it is characterized in that, described aluminium sesquioxide, boron nitride, its particle diameter is 0.2 ~ 1.5 μm of scope.
5., in the preparation method of a kind of silicon nitride ceramics polishing powder according to claim 1, it is characterized in that, described chloric acid cerium: the optimum molar ratio of oxalic acid will between 1:1.5.
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Cited By (4)
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| CN105754489A (en) * | 2016-05-05 | 2016-07-13 | 济南大学 | Preparation method of polishing powder for polishing of emeralds |
| CN105820760A (en) * | 2016-05-05 | 2016-08-03 | 济南大学 | Method for preparing polishing solution used for disk substrate polishing |
| CN105860855A (en) * | 2016-05-05 | 2016-08-17 | 济南大学 | Preparation method of boron nitride composite polishing solution |
| CN105925199A (en) * | 2016-05-05 | 2016-09-07 | 济南大学 | Preparing method of polishing solution for marble |
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| CN105820760A (en) * | 2016-05-05 | 2016-08-03 | 济南大学 | Method for preparing polishing solution used for disk substrate polishing |
| CN105860855A (en) * | 2016-05-05 | 2016-08-17 | 济南大学 | Preparation method of boron nitride composite polishing solution |
| CN105925199A (en) * | 2016-05-05 | 2016-09-07 | 济南大学 | Preparing method of polishing solution for marble |
| CN105820760B (en) * | 2016-05-05 | 2017-10-17 | 济南大学 | A kind of polishing liquid and preparation method thereof polished for magnetic disk substrate |
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