CN104694017B - 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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- CN104694017B CN104694017B CN201510126391.6A CN201510126391A CN104694017B CN 104694017 B CN104694017 B CN 104694017B CN 201510126391 A CN201510126391 A CN 201510126391A CN 104694017 B CN104694017 B CN 104694017B
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- silicon nitride
- polishing
- nitride ceramics
- polishing powder
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- C—CHEMISTRY; METALLURGY
- 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
The present invention relates to a kind of preparing technical field of polishing powder, more particularly to a kind of silicon nitride ceramics polishing powder
Preparation technology and for silicon nitride ceramics polishing in.
Background technology
Silicon nitride is the compound synthesized under artificial condition.Though silicon nitride was just directly synthesized before more than 140 years,
In the memory for staying in people as just the nitride of a kind of stable " infusibility " at that time.After World War II, the rapid of science and technology is sent out
Exhibition, in the urgent need to high temperature resistant, high rigidity, high intensity, erosion-resisting material.Through long-term effort, until nineteen fifty-five silicon nitride
Just it is taken seriously, middle nineteen seventies have just really been obtained high-quality, low cost, there is the silicon nitride ceramics system of extensive important use
Product.
The intensity of silicon nitride is very high, especially hot pressed silicon nitride (HPSN), is one of material most hard in the world.Its extremely resistance to height
Temperature, intensity can maintain to 1200 DEG C of high temperature not decline always, melt body will not be melt into after being heated, until 1900 DEG C of just meetings
Decompose, and have surprising resistance to chemical corrosion, be resistant to almost all of mineral acid and less than 30% soda bath, be also resistant to
The corrosion of many organic acid;It is again simultaneously a kind of high-performance electric insulant.
Silicon nitride is a kind of important structural ceramic material.It is a kind of superhard material, and itself has lubricity, and resistance to
Abrasion, is atomic crystal;Antioxidation during high temperature.And it can also resist thermal shock, more than 1000 DEG C are heated in atmosphere,
Quick refrigeration is drastically heated again, also will not fragmentation.There is so excellent characteristic just because of silicon nitride ceramics, people are usually sharp
The mechanical components such as bearing, blade of gas turbine, mechanical seal ring, permanent mold are manufactured with it.If with high temperature resistant and not
The silicon nitride ceramics for readily conducting heat not only can improve diesel engine quality manufacturing the heating surface of engine components, save fuel, and
And can improve the thermal efficiency.Therefore its polishing process is particularly significant during the smooth silicon nitride ceramics in manufacture surface.
Silicon nitride ceramics production technology includes:Molding → sintering → corase grind → polishing → polishing.Silicon nitride ceramics is thrown
The quality of photoreduction process quality directly affects the quality of its product, thus polishing process in silicon nitride ceramics production process very
Important, polishing powder used directly affects the quality of finish of silicon nitride ceramics in polishing process.
The polishing of silicon nitride ceramics is an extremely complex mechanochemical process.In this process, except machinery work
With outer, also silicon nitride ceramics component, the chemical action between polishing meal component and polished die composition.Therefore, in polishing powder body
In system, the change of chemical composition will cause the adhesion between polished die and silicon nitride ceramics to change, and also cause in work
Regional temperature, polishing powder concentration change, and finally affect polishing efficiency.Therefore, the chemical composition of polishing powder is made pottery to silicon nitride
Porcelain polishing effect is most important.Silicon nitride ceramics hardness relatively spends height, and crystal grain is tiny, uniform.It is highly polished after polishing, so
Polishing powder is needed to have very high hardness when silicon nitride ceramics is processed, it is soft fine and smooth again.
For polishing powder, different polishing powders has different wear intensities.Polishing powder generally by cerium oxide, aluminium oxide,
The components such as silicon oxide, ferrum oxide, zirconium oxide, chromium oxide, stannum oxide are constituted, and the hardness of different materials is different, the change in water
Learn property also different, therefore use occasion is different.The Mohs' hardness of aluminium oxide and chromium oxide is 9, cerium oxide and zirconium oxide
For 7, ferrum oxide is lower.In silicon carbide ceramics polishing process, polishing powder, present people is added all to use chromic oxide mostly
Powder, i.e., be that single polishing powder is polished using single abrasive material, but polishing of this single polishing powder to silicon nitride ceramics reaches not
To excellent polishing effect.Possibly single polishing powder is in polishing friction process.Mobility or soft between the powder of polishing powder
Hardness can not be complementary.Several oxides compounding can overcome the shortcomings of it is above-mentioned, disclosed in Chinese patent application CN101362925B
A kind of compounding polishing powder and preparation method and glossing of polishing optical element, is have 0.5 part~3 parts of chromic oxide
Aluminium sesquioxide composition with 1.0 parts, but the wearability of this compound polishing powder does not reach the polishing requirement of silicon nitride ceramics.
Boron nitride is corrosion-resistant, and very well, generally obtained boron nitride is graphite structure to electrical insulating property, is commonly called as white stone
Ink.Another kind is diamond-type, similar with the principle that graphite is changed into diamond, graphite mould boron nitride high temperature (1800 DEG C),
Buddha's warrior attendant type boron nitride can be changed under high pressure (8000Mpa) [5~18GPa].It is the superhard material of novel fire resistant, Mohs' hardness
More than 10, its epigranular, hardness are high, self-sharpening is strong, and cutting power is stronger, stable chemical nature, and heat conductivity is good.The application will
Boron nitride prepares a kind of polishing powder for silicon nitride ceramics polishing with rare earth oxide, chromium oxide, and the polishing powder has hardness
The advantages of high, good fluidity and heat conductivity are good, soft durometer can not be complementary.
The content of the invention
The mesh of the present invention is to provide one kind and can reduce polishing cut, improve polishing powder gouge hardness, improves silicon nitride ceramics
The preparation method and technology of the polishing powder of fineness;
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of silicon nitride ceramics polishing powder, is characterised by that the method has following processing step:In reaction
In device, 8%~11% cerium chloride, 28%~38% chromic acid, 2%~5% dodecyl are added by mass percentage
Benzene sulfonic acid sodium salt is dissolved in the water, and adds 10%~20% aluminium sesquioxide, 32%~45% boron nitride, and stirring is in slurry
Liquid, then 3%~8% dissolving oxalic acid is added after water, each component sum is for absolutely, water is not counted in component, under normal pressure, stirs
Mix, add 85 DEG C of heat, react 18~24h, make cerium chloride generate evengranular Sedemesis., solid-liquid separation, 1100 DEG C~
1150 DEG C of 5~8h of roasting, after cooling, Jing comminution by gas stream obtains final product silicon nitride ceramics polishing powder, resulting silicon nitride ceramics polishing
The particle diameter of powder is in the range 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 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 exists
0.2~1.5 μ m.
In a kind of preparation method of silicon nitride ceramics polishing powder, described chloric acid cerium:The optimum molar ratio of oxalic acid will be
1:1.5 between.
In a kind of preparation method of silicon nitride ceramics polishing powder, the effect of oxalic acid is to make cerium chloride generate Sedemesis. precipitation
The surface of solid phase is attached to, excessive oxalic acid passes through heat resolve to product without impact.
Particle size test method of the present invention is the granularity equivalent diameter size measured using laser particle analyzer.
Silicon nitride ceramics polishing powder method obtained by the present invention:Can be used for wet throwing and can also be used for dry throwing, per square
Rice consumption is 15~20g.
The present invention compared with the prior art, has the advantage that and beneficial effect:
(1) present invention obtains silicon nitride ceramics polishing powder, in preparation process, using boron nitride component is added, makes polishing
The polishing gouge hardness of powder is significantly improved, and can be used for the polishing of various high hardness silicon nitride ceramics.
(2) present invention obtains silicon nitride ceramics polishing powder, and in preparation process, addition oxalic acid is precipitant, and oxalic acid is adding
Decomposing oxalic acid root in thermal process, the concentration for making system oxalate unanimously generates Sedemesis. for precipitation from homogeneous solution system with cerium chloride,
So form Sedemesis. granule tiny and uniform.Chromic acid, Sedemesis. generate cerium oxide, chromic oxide after sintering
Granule fine uniform is distributed on aluminium sesquioxide, nitridation boron surface, particle size distribution narrow spy little with meso-position radius grain
Point, while making between the powder of polishing powder that mobility or soft durometer are complementary, reaches more preferable polishing effect.
(3) present invention obtains silicon nitride ceramics polishing powder, and preparation process is simple, condition is easily controllable, low production cost, easily
In industrialized production.
Specific embodiment
Embodiment 1
A kind of preparation method of silicon nitride ceramics polishing powder, in the reactor, is separately added into the cerium chloride of 9g, and the three of 32g
Chromium oxide, 3g dodecylbenzene sodium sulfonate is dissolved in the water, and adds the aluminium sesquioxide of 15g, the boron nitride of 36g, and stirring is in
Serosity, then 5g dissolving oxalic acids are added after water, water is not counted in component, and under normal pressure, stirring adds 85 DEG C of heat, reacts 21h, makes
The evengranular Sedemesis. of cerium chloride generation, solid-liquid separation, in 1100 DEG C of roasting 6h, after cooling, Jing comminution by gas stream obtains final product nitridation
The ceramic polished powder of silicon, the particle diameter of resulting silicon nitride ceramics polishing powder is in the range of 0.2~2.0 μm.
Embodiment 2
A kind of preparation method of silicon nitride ceramics polishing powder, in the reactor, is separately added into the cerium chloride of 8g, and the three of 36g
Chromium oxide, 2g dodecylbenzene sodium sulfonate is dissolved in the water, and adds the aluminium sesquioxide of 12g, the boron nitride of 38g, and stirring is in
Serosity, then 4g dissolving oxalic acids are added after water, water is not counted in component, and under normal pressure, stirring adds 85 DEG C of heat, reacts 18h, makes
The evengranular Sedemesis. of cerium chloride generation, solid-liquid separation, in 1150 DEG C of roasting 7h, after cooling, Jing comminution by gas stream obtains final product nitridation
The ceramic polished powder of silicon, the particle diameter of resulting silicon nitride ceramics polishing powder is in the range of 0.2~2.0 μm.
Embodiment 3
A kind of preparation method of silicon nitride ceramics polishing powder, in the reactor, is separately added into the cerium chloride of 11g, and the three of 28g
Chromium oxide, 4g dodecylbenzene sodium sulfonate is dissolved in the water, and adds the aluminium sesquioxide of 10g, the boron nitride of 41g, and stirring is in
Serosity, then 6g dissolving oxalic acids are added after water, water is not counted in component, and under normal pressure, stirring adds 85 DEG C of heat, reacts 22h, makes
The evengranular Sedemesis. of cerium chloride generation, solid-liquid separation, in 1130 DEG C of roasting 8h, after cooling, Jing comminution by gas stream obtains final product nitridation
The ceramic polished powder of silicon, the particle diameter of resulting silicon nitride ceramics polishing powder is in the range of 0.2~2.0 μm.
Embodiment 4
A kind of preparation method of silicon nitride ceramics polishing powder, in the reactor, is separately added into the cerium chloride of 10g, and the three of 30g
Chromium oxide, 5g dodecylbenzene sodium sulfonate is dissolved in the water, and adds the aluminium sesquioxide of 18g, the boron nitride of 32g, and stirring is in
Serosity, then 5g dissolving oxalic acids are added after water, water is not counted in component, and under normal pressure, stirring adds 85 DEG C of heat, reacts 23h, makes
The evengranular Sedemesis. of cerium chloride generation, solid-liquid separation, in 1140 DEG C of roasting 5h, after cooling, Jing comminution by gas stream obtains final product nitridation
The ceramic polished powder of silicon, the particle diameter of resulting silicon nitride ceramics polishing powder is in the range of 0.2~2.0 μm.
Embodiment 5
A kind of preparation method of silicon nitride ceramics polishing powder, in the reactor, is separately added into the cerium chloride of 9g, and the three of 38g
Chromium oxide, 2g dodecylbenzene sodium sulfonate is dissolved in the water, and adds the aluminium sesquioxide of 13g, the boron nitride of 34g, and stirring is in
Serosity, then 4g dissolving oxalic acids are added after water, water is not counted in component, and under normal pressure, stirring adds 85 DEG C of heat, reacts 24h, makes
The evengranular Sedemesis. of cerium chloride generation, solid-liquid separation, in 1130 DEG C of roasting 6.5h, after cooling, Jing comminution by gas stream obtains final product nitrogen
The ceramic polished powder of SiClx, the particle diameter of resulting silicon nitride ceramics polishing powder is in the range of 0.2~2.0 μm.
Embodiment 6
A kind of preparation method of silicon nitride ceramics polishing powder, in the reactor, is separately added into the cerium chloride of 8g, and the three of 34g
Chromium oxide, 3g dodecylbenzene sodium sulfonate is dissolved in the water, and adds the aluminium sesquioxide of 10g, the boron nitride of 42g, and stirring is in
Serosity, then 3g dissolving oxalic acids are added after water, water is not counted in component, and under normal pressure, stirring adds 85 DEG C of heat, reacts 19h, makes
The evengranular Sedemesis. of cerium chloride generation, solid-liquid separation, in 1150 DEG C of roasting 7.5h, after cooling, Jing comminution by gas stream obtains final product nitrogen
The ceramic polished powder of SiClx, the particle diameter of resulting silicon nitride ceramics polishing powder is in the range of 0.2~2.0 μm.
Using method:Can be used for wet throwing and can also be used for dry throwing, polishing powder and water are tuned into into starchiness during wet throwing, it is proposed that
From wet throwing, because dry polishing powder dirt can be polluted.
The present invention obtains silicon nitride ceramics polishing powder, and powder body polishing effect is good, glossiness, reachable more than 99 degree, no marking,
Flatness is high, and the consumption of powder is few.
Claims (4)
1. a kind of preparation method of silicon nitride ceramics polishing powder, is characterised by that the method has following processing step:In reactor
In, 8%~11% cerium chloride, 28%~38% chromic acid, 2%~5% detergent alkylate are added by mass percentage
Sodium sulfonate is dissolved in the water, and adds 10%~20% aluminium sesquioxide, 32%~45% Buddha's warrior attendant type boron nitride, and stirring is in
Serosity, then 3%~8% dissolving oxalic acid is added after water, each component sum is a hundred per cent, and water is not counted in component, under normal pressure,
Stirring, is heated to 85 DEG C, reacts 18~24h, makes cerium chloride generate evengranular Sedemesis., solid-liquid separation, 1100 DEG C~
1150 DEG C of 5~8h of roasting, after cooling, Jing comminution by gas stream obtains final product silicon nitride ceramics polishing powder, resulting silicon nitride ceramics polishing
The particle diameter of powder is in the range of 0.2~2.0 μm.
2. a kind of preparation method of silicon nitride ceramics polishing powder according to claim 1, it is characterised in that described cerium chloride
For anhydrous cerium chloride.
3. a kind of preparation method of silicon nitride ceramics polishing powder according to claim 1, it is characterised in that three described oxidations
Two aluminum, Buddha's warrior attendant type boron nitride, its particle diameter is in 0.2~1.5 μ m.
4. a kind of preparation method of silicon nitride ceramics polishing powder according to claim 1, it is characterised in that described chlorination
Cerium:The optimum molar ratio of oxalic acid will be 1:1.5 between.
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