CN109483420A - A kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing - Google Patents

A kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing Download PDF

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Publication number
CN109483420A
CN109483420A CN201811478625.3A CN201811478625A CN109483420A CN 109483420 A CN109483420 A CN 109483420A CN 201811478625 A CN201811478625 A CN 201811478625A CN 109483420 A CN109483420 A CN 109483420A
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China
Prior art keywords
mixing
ultra
carbon dioxide
supercritical fluid
autoclave
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CN201811478625.3A
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Chinese (zh)
Inventor
刘宾
王志起
李鹤南
席耀辉
王朝富
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Zhengzhou Research Institute for Abrasives and Grinding Co Ltd
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Zhengzhou Research Institute for Abrasives and Grinding Co Ltd
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Priority to CN201811478625.3A priority Critical patent/CN109483420A/en
Publication of CN109483420A publication Critical patent/CN109483420A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D18/00Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
    • B24D18/009Tools not otherwise provided for

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Polishing Bodies And Polishing Tools (AREA)

Abstract

A kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing, include the following steps: (1) according to weight percent be abrasive material 25~50%, vitrified bond 4~26%, wetting agent 1~25% first by abrasive material, vitrified bond and wetting agent be added autoclave in, sealing;(2) carbon dioxide is injected into autoclave, and pressure and temperature is adjusted to 72.8 atm, 31.1 DEG C or more respectively, and carbon dioxide is made to reach supercriticality;Stir 1 ~ 3h.For in ultra-fine grinding tool preparation process, because the problem that powder surface higher can easily reunite is studied, the gap of aggregate is sufficiently infiltrated using the extremely strong supercritical fluid carbon dioxide of penetrating power, achieve the purpose that weaken the binding force between particle, solves the problems, such as that each component reunion conventional method is difficult to open in ultra-fine grinding tool preparation process;Also solve the problems, such as that mixture process is complicated in conventional mixing procedure and is easily segregated simultaneously.

Description

A kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing
Technical field
The invention belongs to grinding tool preparation technical fields, and in particular to a kind of Ultra-fine ceramic abrasive tool supercritical fluid mixing Method.
Background technique
Vitrified bonded grinding tool has that grinding capacity is strong, shape retention is good, grinding accuracy is high, is not easy to plug and work of burning Part, easily finishing and a series of excellent performances such as high temperature-resistant acid-resistant alkali can adapt to the grinding and various processing essence of various coolant liquids Desired grinding is spent, thus is most widely used.Ultra-fine grinding wheel (grinding wheel solid granularity is lower than 5 μm) is made in some products For last one of technique, processing quality directly determines the yields of product, therefore, stability and mill of the user to ultra-fine grinding tool Cut quality requirement continuous improvement.Since component powder granularity is meticulous in ultra-fine grinding tool, own face can be high, each component in mixing Reunion be difficult to open, eventually lead to that grinding tool interior tissue and hardness are uneven, and grinding wheel viscous bits often occurs, burns, grinding efficiency The occurrence of low, the grinding quality and stability of such grinding tool are far below import similar product.Ultra-fine is improved at present The uniformity conventional method of molding mass, one side process flow is complicated, and it is longer to expend the time;On the other hand it is easily introduced impurity, is Grinding tool performance brings uncontrollable factor.
Its density of supercritical carbon dioxide is bordering on liquid, and viscosity is bordering on gas, diffusion coefficient 10−4 cm2 s−1, much higher than general Logical liquid.Therefore, supercritical carbon dioxide has extremely strong penetrating power, easily diffuses into the gap between particle In, weaken the bond strength between agglomerated particle.It is radial due to existing in barrel meanwhile in high speed agitator whipping process Velocity gradient, the agglomerated particle in slurry is by the strong shear perpendicular to radial direction.Particle in high-frequency collision, squeeze, cut Under the collective effect cut, the dough of reunion is gradually removed, by until breaing up completely.It is overcritical during dough depolymerization The wetting agent dissolved in carbon dioxide is sufficiently wrapped in each particle surface, plays the effect of its steric hindrance, can be in gas-solid point From secondary agglomeration, the segregation for effectively preventing particle in the process.
On the one hand supercritical fluid method for mixing improves the efficiency of the uniform mixing of superfine powder, while solving conventional mixing side Formula process is complicated and the problem being segregated easily occurs.
Summary of the invention
The purpose of the present invention is to provide a kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing.
Based on above-mentioned purpose, the present invention is adopted the following technical scheme that:
A kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing, includes the following steps:
It (1) is abrasive material 25~50%, vitrified bond 4~26%, wetting agent 1~25% first by abrasive material, pottery according to weight percent Porcelain bonding agent and wetting agent are added in autoclave, sealing;
(2) carbon dioxide is injected into autoclave, and pressure and temperature is adjusted to 72.8 atm, 31.1 DEG C or more respectively, makes two Carbonoxide reaches supercriticality;Stir 1 ~ 3h;
(3) after mixing, decompression makes supercritical carbon dioxide be converted into gas, and discharges, and mixing is taken out after being cooled to room temperature Material.
Further, abrasive material is any one of diamond, cubic boron nitride, corundum, silicon carbide and silica or two The mixture of kind any of the above ratio, abrasive grain are 0.01 μm~5 μm.
The wetting agent is the mixture of one or more of paraffin, stearic acid and propolis arbitrary proportion.
The vitrified bond can be well known vitrified bond commonly used in the art, such as vitrified bond, crystallite glass Glass bonding agent, conventional ceramic bonding agent ceramics, the granularity of the vitrified bond is 0.01 μm~5 μm.
Detailed process is as follows for step (2): being passed through carbon dioxide into autoclave to drain the air in autoclave;By air inlet After mouth valve is fastened, heating;When temperature reaches 45 ~ 95 °, injection carbon dioxide makes pressure reach 8 ~ 12MPa.
When the air-discharging, 1 ~ 3L/min of carbon dioxide flow, being passed through the time continues 30 ~ 60s.
It can also be added in step (1) of the present invention to adjust the polar dressing agent of supercritical carbon dioxide, the dressing agent For the mixture of one or more of carbon disulfide, ethyl alcohol and hexane arbitrary proportion, the vitrified bond and modification The mass ratio of agent is 1 ︰ (0.5 ~ 2).
The present invention does not have special restriction to the mixed mode, using hybrid mode well known to those skilled in the art , specifically, such as kettle heat.
For in ultra-fine grinding tool preparation process, because the problem that powder surface higher can easily reunite is studied, benefit The gap that aggregate is sufficiently infiltrated with the extremely strong supercritical fluid carbon dioxide of penetrating power reaches the combination between reduction particle The purpose of power solves the problems, such as that each component reunion conventional method is difficult to open in ultra-fine grinding tool preparation process;Simultaneously Solve the problems, such as that mixture process is complicated in conventional mixing procedure and is easily segregated.
Ultra-fine grinding tool each component is uniformly mixed, and abrasive article structures are uniform, hardness is consistent, occur when effectively reducing grinding viscous bits, The occurrence of burn, grinding efficiency are low etc., it is effective to improve grinding performance and processing quality.
Detailed description of the invention
Fig. 1 is the scanning electron microscope microphoto after 1 supercritical liq mixing of embodiment;
Fig. 2 is the scanning electron microscope microphoto after 4 supercritical liq mixing of embodiment;
Fig. 3 is the scanning electron microscope microphoto after 5 supercritical liq mixing of embodiment.
Specific embodiment
Below in conjunction with specific embodiment, further details of the technical solution of the present invention, but protection model of the invention It encloses and is not limited thereto.
Embodiment 1
A kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing, the specific steps are as follows:
(1) by 4.5 μm of diamond 26g, 2 μm of vitrified bond 6g, paraffin 8g are added in 1L autoclave, seal;
(2) carbon dioxide is passed through into autoclave to drain the air in autoclave, carbon dioxide flow 2L/min, time 45s; After inlet port valve door closure, heating;When temperature reaches 95 °, injecting a certain amount of carbon dioxide by booster makes pressure Reach 8MPa;
(3) blender is started, revolving speed is adjusted to 1200 rpm, under the action of supercritical fluid, sufficiently opens the group of each material It is poly-, and by the paraffin uniform adsorption being dissolved in supercritical fluid in each surface of material, mixing time continues 1 h;
(4) after mixing, control valve is opened, decompression makes supercritical carbon dioxide be converted into gas, and discharges, and is cooled to room temperature Mixture is taken out afterwards.
The microphoto of mixture after above method mixing is as shown in Figure 1, the equal soilless sticking of mixture each component, each component Material is evenly distributed.
Embodiment 2
A kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing, the specific steps are as follows:
(1) by 3.5 μm of 32g silicon carbide, 1.5 μm of devitrified glass bonding agent 6g, stearic acid 10g is added in 1L autoclave, close Envelope;
(2) carbon dioxide is passed through into autoclave to drain the air in kettle, carbon dioxide flow 2L/min, time 45s;It will be into After port valve is fastened, heating, when temperature reaches 95 °, injecting a certain amount of carbon dioxide by booster reaches pressure 8MPa;
(3) blender is started, revolving speed is adjusted to 1200 rpm, under the action of supercritical fluid, sufficiently opens the group of each material It is poly-, and by the paraffin uniform adsorption being dissolved in supercritical fluid in each surface of material, mixing time continues 1 h;
(4) after mixing, control valve is opened, decompression makes supercritical carbon dioxide be converted into gas, and discharges, and is cooled to room temperature Mixture is taken out afterwards.
The equal soilless sticking of gained mixture each component, each group sub-material are evenly distributed.
Embodiment 3
A kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing, the specific steps are as follows:
(1) by 3.5 μm of 38g white fused alumina, 0.5 μm of conventional ceramic bonding agent 8g, propolis 14g are added in 1L autoclave, sealing;
(2) carbon dioxide is passed through into autoclave to drain the air in kettle, carbon dioxide flow 2L/min, time 45s;It will be into After port valve is fastened, heating, when temperature reaches 45 °, injecting a certain amount of carbon dioxide by booster reaches pressure 12MPa。
(3) blender is started, revolving speed is adjusted to 1200 rpm, under the action of supercritical fluid, sufficiently opens each material Reunion, and by the propolis uniform adsorption being dissolved in supercritical fluid in each surface of material, mixing time continues 1 h;
(4) after mixing, control valve is opened, decompression makes supercritical carbon dioxide be converted into gas, and discharges, and is cooled to room temperature Mixture is taken out afterwards.
The equal soilless sticking of gained mixture each component, each group sub-material are evenly distributed.
Embodiment 4
A kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing, the specific steps are as follows:
(1) by 1 μm of 18g white fused alumina, 2.5 μm of silica 4g, 4.5 μm of diamond 20g, 0.5 μm of conventional ceramic bonding agent 5g, propolis 8g, ethyl alcohol 5g are added in 1L autoclave, sealing;
(2) carbon dioxide is passed through into autoclave to drain the air in kettle, carbon dioxide flow 2L/min, time 45s;It will be into After port valve is fastened, heating, when temperature reaches 45 °, injecting a certain amount of carbon dioxide by booster reaches pressure 12MPa;
(3) blender is started, revolving speed is adjusted to 1200 rpm, under the action of supercritical fluid, sufficiently opens the group of each material It is poly-, and by the propolis uniform adsorption being dissolved in supercritical fluid in each surface of material, mixing time continues 2 h;
(4) after mixing, control valve is opened, decompression makes supercritical carbon dioxide be converted into gas, and discharges, and is cooled to room temperature Mixture is taken out afterwards.
The microphoto of mixture after above method mixing is as shown in Fig. 2, the equal soilless sticking of gained mixture each component, each Component material is evenly distributed.
Embodiment 5
A kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing, the specific steps are as follows:
(1) by 4.5 μm of 18g diamond, by 0.5 μm of 10g silicon carbide, by 0.1 μm of 7.5g white fused alumina, 0.1 μm of crystallite Glass ceramics bonding agent 8g, stearic acid 2g, paraffin 6g are added in 1L autoclave, seal;
(2) carbon dioxide is passed through into autoclave to drain the air in kettle, carbon dioxide flow 2L/min, time 45s;It will be into After port valve is fastened, heating, when temperature reaches 95 °, injecting a certain amount of carbon dioxide by booster reaches pressure 8MPa;
(3) blender is started, revolving speed is adjusted to 2000 rpm, under the action of supercritical fluid, sufficiently opens the group of each material It is poly-, and by the paraffin being dissolved in supercritical fluid and stearic acid uniform adsorption in each surface of material, mixing time continues 2 h;
(4) after mixing, control valve is opened, decompression makes supercritical carbon dioxide be converted into gas, and discharges, and is cooled to room temperature Mixture is taken out afterwards.
The microphoto of mixture after above method mixing is as shown in figure 3, the equal soilless sticking of gained mixture each component, each Component material is evenly distributed.
Grinding wheel, and the grinding to grinding wheel is made according to conventional method in that art in the mixture obtained using above-mentioned method for mixing Performance is detected, as a result as follows:
As seen from the above table, the uniformity of hardness of the grinding wheel prepared using mixture of the invention improves 73.8 ~ 96.4%, hardness Unanimously, the performance of grinding wheel is improved.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (6)

1. a kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing, which comprises the steps of:
(1) according to abrasive material, vitrified bond and wetting agent weight ratio, ((4 ~ 26) ︰ (1 ~ 25) are by abrasive material, Ceramic bond by 25 ~ 50) ︰ Agent and wetting agent are added in autoclave, sealing;
(2) carbon dioxide is injected into autoclave, and pressure and temperature is adjusted to 72.8 atm, 31.1 DEG C or more respectively, makes two Carbonoxide reaches supercriticality;1 ~ 3h of stir mixing;
(3) after mixing, decompression makes supercritical carbon dioxide be converted into gas, and discharges, and mixing is taken out after being cooled to room temperature Material.
2. Ultra-fine ceramic abrasive tool supercritical fluid method for mixing according to claim 1, which is characterized in that abrasive material is gold The mixture of any one of hard rock, cubic boron nitride, corundum, silicon carbide and silica or two or more arbitrary proportions, mill Material granularity is 0.01 μm~5 μm.
3. Ultra-fine ceramic abrasive tool supercritical fluid method for mixing according to claim 1, which is characterized in that the wetting Agent is the mixture of one or more of paraffin, stearic acid and propolis arbitrary proportion.
4. Ultra-fine ceramic abrasive tool supercritical fluid method for mixing according to claim 1, which is characterized in that the ceramics The granularity of bonding agent is 0.01 μm~5 μm.
5. Ultra-fine ceramic abrasive tool supercritical fluid method for mixing according to claim 1, which is characterized in that step (2) Detailed process is as follows: being passed through carbon dioxide into autoclave to drain the air in autoclave;After inlet port valve door closure, add Heat;When temperature reaches 45 ~ 95 °, injection carbon dioxide makes pressure reach 8 ~ 12MPa.
6. Ultra-fine ceramic abrasive tool supercritical fluid method for mixing according to claim 5, which is characterized in that the emptying When gas, 1 ~ 3L/min of carbon dioxide flow, being passed through the time continues 30 ~ 60s.
CN201811478625.3A 2018-12-05 2018-12-05 A kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing Pending CN109483420A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112427646A (en) * 2020-12-02 2021-03-02 山东理工大学 Method for preparing magnetic abrasive material by supercritical carbon dioxide assisted plasma spray

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CN101870091A (en) * 2010-06-17 2010-10-27 大连理工大学 Method for preparing ultra-fine diamond grinding wheel of vitrified bond
CN102499238A (en) * 2011-11-25 2012-06-20 北京化工大学常州先进材料研究院 Method for preparing sustained-release insecticide microcapsule by using supercritical fluid technology
CN105619266A (en) * 2015-12-23 2016-06-01 郑州磨料磨具磨削研究所有限公司 Low-temperature sintering ceramic binding agent, grinding wheel and preparation method thereof
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Publication number Priority date Publication date Assignee Title
CN112427646A (en) * 2020-12-02 2021-03-02 山东理工大学 Method for preparing magnetic abrasive material by supercritical carbon dioxide assisted plasma spray

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