WO2005042661A1 - セリウム系研摩材及びセリウム系研摩材の製造方法 - Google Patents
セリウム系研摩材及びセリウム系研摩材の製造方法 Download PDFInfo
- Publication number
- WO2005042661A1 WO2005042661A1 PCT/JP2004/014197 JP2004014197W WO2005042661A1 WO 2005042661 A1 WO2005042661 A1 WO 2005042661A1 JP 2004014197 W JP2004014197 W JP 2004014197W WO 2005042661 A1 WO2005042661 A1 WO 2005042661A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- lanthanum
- abrasive
- cerium
- particles
- slurry
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C19/00—Surface treatment of glass, not in the form of fibres or filaments, by mechanical means
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
Definitions
- the present invention relates to a cerium-based abrasive containing rare earth element compound particles such as cerium oxide particles as a main component, and more particularly to an abrasive containing lanthanum and a method for producing the same.
- Cerium-based abrasives (hereinafter also simply referred to as abrasives) have conventionally been widely used as abrasives for glass.
- glass substrates have been used as substrates for electronic materials, such as glass for magnetic recording media such as hard disks and glass substrates for liquid crystal displays (LCDs). Tepuru.
- Abrasive materials are required to have an abrasive force and maintain it so that the abrasive operation can be performed efficiently.
- a fluorine component may be added to the abrasive in order to improve the abrasive power.
- a fluorine component may be added to the abrasive in order to improve the abrasive power.
- highly basic lanthanum can be partially neutralized with fluorine, and further, glass can be further neutralized.
- a type of hydrated erosion layer is formed, which promotes polishing by forming ky fluoride.
- the light rare earth material is fluorinated with hydrofluoric acid, and by setting the fluorine content to 3 to 9%, it is possible to obtain an abrasive having high abrasive power for a long period of time.
- Patent Document 1 JP-A-9-183966
- Abrasives containing such a fluorine component may not be preferable from the viewpoint of recycling. That is, a post-treatment of removing used components from the used abrasive is required, and the handling may be complicated.
- high-cerium abrasives having an increased cerium oxide content in the abrasives have been developed as abrasives which do not require the addition of a fluorine component while maintaining the abrasive power.
- this high cerium abrasive is not without problems. This is because a raw material made of high-purity cerium carbonate or the like is used, but excessive particle growth occurs in the roasting step, which causes coarse particles. And since the generation of coarse particles causes polishing scratches, after roasting It is important to apply the pulverizing step and the classification step, but if the coarse particles are excessively generated, the load on the post-roasting step is increased, and efficient production cannot be performed.
- the present invention has been made in view of the above background, and provides a cerium-based abrasive excellent in abrasive power while eliminating the need for addition of a fluorine component. It is an object to provide a method for manufacturing a material.
- lanthanum conjugate particles particles containing lanthanum as a main component
- the lanthanum conjugate particles are generated in the process of producing the abrasive, and are generated in the following process. That is, in the process of producing an abrasive using lanthanum-containing rare earth carbonate or the like as a raw material, cerium oxide forms a composite oxide while taking in the lanthanum component in the roasting step, and this composite oxide is polished. Become particles. Then, the roasted product after roasting is slurried and subjected to a wet treatment such as wet pulverization to adjust the abrasive particles to a predetermined particle size. Part of the incorporated lanthanum component elutes and reacts with the solvent to produce lanthanum compound particles (see JP-A-2004-123889).
- the lanthanum conjugate particles have a hydroxide as a main component. According to the present inventors, it is considered that the lanthanum compound particles exist in a state in which they are free from the abrasive particles, but in some cases they are attached to the surface of the abrasive particles.
- the present inventors have studied the relationship between the lanthanum ligature particles and the abrasive force. It was. As a result, they have found that an abrasive having a low lanthanum ligature content, particularly an abrasive having a low lanthanum ligature content on the surface of the abrasive particles, has excellent abrasive power. Therefore, the present inventors have arrived at the present invention based on the above findings assuming that there is a cerium-based abrasive containing lanthanum, which has a high abrasive power, and particularly has a good ability to hold the abrasive power.
- the present invention provides a cerium-based abrasive containing lanthanum, in which the CeZLa element ratio (S) on the surface of the abrasive particles is larger than the CeZLa element ratio (B) of the entire abrasive particles (S> B).
- S CeZLa element ratio
- B CeZLa element ratio
- the abrasive according to the present invention has reduced lanthanum compound particles that cause a reduction in abrasive power on the abrasive particle surface. Therefore, according to the present invention, an efficient polishing operation can be performed while ensuring the polishing force. Further, in the present invention, excessive grain growth of the abrasive particles during the roasting step due to the action of lanthanum is suppressed in the production process. Therefore, according to the present invention, a highly accurate polished surface can be formed.
- the relationship between the CeZLa element ratio (S) on the surface of the polishing particles and the CeZLa element ratio (B) on the entire polishing particles is represented by a force required to satisfy S> 1.
- OB Preferably, S ⁇ l. It is preferable to use 05B.
- the upper limit is preferably S ⁇ 5 OB. If the SZB value is too large, the cerium grade of the surface layer of the particles is high, so that the initial polishing force is high, but the cerium grade inside the particles is low, so that the sustainability of the polishing force may be poor.
- the CeZLa element ratio of the whole abrasive particles is preferably 3Z7-9Z1.
- the content of lanthanum is greater than 9/1, the grain growth is likely to occur in the abrasive production process. If the content of lanthanum is less than 3Z7, the content of lanthanum is less than that of the abrasive. Cerium, which has an effective effect, is too small to cause a decrease in polishing power.
- the present invention reduces the lanthanum component, which is considered to be a cause of various problems affecting the polishing force, such as clogging of a nod that occurs during the polishing process, in the surface portion of the polishing particles.
- the fluorine content in the present invention is preferably 3% by weight or less.
- a method for measuring the CeZLa element ratio of the whole abrasive particles a method in which the abrasive is alkali-melted and the solution analysis is performed is preferable.
- a composition analysis method is preferably ICP (inductively coupled plasma emission). Spectroscopy) is preferred.
- XPS X-ray photoelectron spectroscopy
- the average particle size of the abrasive particles is, for example, 0.1 m or more and 3.0 m or less in a force that can take various sizes depending on the application and the like. Is preferred. If the average particle size of the agglomerated particles is less than 0.1 ⁇ m, sufficient abrasive power cannot be given to the abrasive and the required polishing rate cannot be secured. On the other hand, if the average particle size is larger than 3. O / zm, it becomes difficult to perform precise polishing.
- the method for producing a cerium-based abrasive according to the present invention is the same as the conventional process for producing a cerium-based abrasive except that a step of removing lanthanum ligated particles is added.
- the conventional cerium-based abrasives include a pre-treatment step of pulverizing the abrasive raw material, a roasting step of roasting the pre-treated raw material to form abrasive particles mainly composed of cerium oxide, and a post-roasting step.
- a material having a low fluorine content is preferred. It is preferable to use a material which does not contain fluorine such as rare earth and contains a rare earth element in a high ratio. However, even if it is a nostonesite concentrate, it can be applied as long as the fluorine content can be reduced, for example, by mixing with rare earth carbonate. Here, it is preferable that the fluorine content of the abrasive material is 3% by weight or less.
- LOI Loss on Ignition
- the pretreatment step is a step to be performed before roasting, and is basically based on a step of pulverizing raw materials. If necessary, an alkali metal such as sodium which causes abnormal grain growth during roasting is removed. This includes a chemical treatment step of adding a mineral acid for removal, a step of drying the raw material pulverized before roasting, and the like.
- the roasting temperature in the roasting step is a force that requires a temperature of 500 ° C or more to form a complex oxidized product (solid solution) of cerium and lanthanum.
- the polishing force of the abrasive is maintained.
- Is preferably roasted at a temperature of 800-1200 ° C.
- the intermediate raw material after the roasting which is the object of the wet grinding, has a CeZLa ratio of 3Z7-9Z1. If the content of lanthanum is small, lanthanum compound particles are less likely to be generated in the subsequent wet grinding step, and the effect of the present invention is less likely to be exhibited. If the content of lanthanum is large, particles having a lanthanum compound power are easily generated, but the content of cerium is reduced, so that the abrasive material has a low V and a polishing rate.
- wet grinding As wet treatment after roasting, wet grinding is usually shown. In this wet milling, the abrasive particles are powdered into smaller abrasive particles, and at the same time, the lanthanum component flows out of the abrasive particles due to a mechanochemical reaction, and particles forming a lanthanum compound are generated on the surface side. It will be easier.
- the wet treatment includes wet classification as well as wet pulverization.
- the lanthanum conjugate particles are generated in the wet processing step, the removal is performed on the roasted product after the wet processing.
- the lanthanum conjugate particles in the roasted product slurry after the wet treatment are considered to be mainly composed of a hydroxide. Further, when the roasted product after the wet treatment is dried, it is considered that the lanthanum ligature particles contain the acid ligne.
- a method of removing the lanthanum compound particles from the roasted material after the wet treatment a method in which the roasted material is brought into contact with a lanthanum hydroxide or a solution in which the lanthanide is soluble is preferable.
- a solution in which the hydroxide and the acid-soluble substance are soluble include an acid or a chelating agent.
- the acid a mineral acid such as sulfuric acid, hydrochloric acid, or nitric acid is preferable in terms of cost. Organic acids such as DTA and citric acid or salts thereof are preferred.
- the lanthanum ligature particles may be removed by adding a mineral acid and a chelating agent in any combination.
- Hydrofluoric acid is a mineral acid such as lanthanum hydroxide or lanthanum fluoride, which is considered to be water-insoluble lanthanum fluoride and cannot be used alone because it cannot reduce the lanthanum component on the surface of the abrasive particles. Is not preferred.
- a mineral acid chelating agent other than hydrofluoric acid for example, after removing a lanthanum hydroxide or a lanthanide shading agent with a mineral acid chelating agent other than hydrofluoric acid, Addition of hydrofluoric acid with a fluorine concentration of 3% or less can be implemented as an application of the present invention.
- the removal of the lanthanum compound particles may be performed by drying the slurry after the wet treatment, collecting the roasted product, and bringing the roasted product into contact with a solution in which the lanthanum hydroxide or lanthanum sulfide is soluble.
- a preferred method is to add a solution in which the lanthanum hydroxide or the lanthanum hydroxide is soluble to the slurry after the wet treatment. This is because the lanthanum ligature particles can be removed immediately after the wet treatment, and the number of steps can be reduced.
- the amount of the solution such as a mineral acid is controlled by controlling the pH of the slurry at the time of addition. Do more. Specifically, it is preferable to add the solution until the pH of the slurry becomes 5 or less. This is because when the pH is 5 or less, the lanthanum conjugate particles can be dissolved.
- the dissolution treatment of the particles of the lanthanum conjugate may be performed after the wet treatment, or the dissolution treatment as described above may be performed in parallel during the wet treatment.
- praseodymium like lanthanum
- the abrasive may precipitate on the surface of the abrasive particles in the wet processing step, and may dissolve the surface of the abrasive particles by dissolution treatment.
- the slurry after the dissolution treatment of the lanthanum compound particles can be used as it is as an abrasive slurry since the lanthanum conjugate particles have disappeared.
- the cerium-based abrasive according to the present invention has a high abrasive power without containing fluorine, and enables efficient abrasive work. And since it does not need to contain fluorine, it is possible to recycle used abrasives. Therefore, it is possible to effectively use a rare earth element having added value such as cerium.
- the abrasive according to the present invention can be manufactured only by adding a step of adding a solution such as a mineral acid to the roasted material after the wet treatment. Method.
- First Embodiment II A rare earth carbonate containing cerium and lanthanum at an elemental ratio of 60:40 and containing 0.5% by weight or less of fluorine was prepared as a cerium-based abrasive material. Then, this raw material is dispersed in pure water at a mass ratio of 1: 2 to prepare a slurry, and the average particle diameter D after pulverization is 1.0 m using a bead mill (pulverization medium is 0.4 mm in diameter). Go crushing
- the pulverized particles obtained by filtering this slurry were dried at 120 ° C. for 24 hours.
- the dried pulverized particles were roasted in an electric furnace at 900 ° C for 8 hours to obtain a rare earth oxide powder (roasted product), and the obtained powder was released to room temperature. Cooled down.
- this raw material and pure water were mixed at a mass ratio of 1: 2 to prepare a slurry, and pulverization was performed using a bead mill (diameter of the pulverization medium: 0.8 mm).
- the average particle size of the pulverized particles in the obtained slurry was measured using a particle size distribution analyzer, the average particle size D was 0.8 m.
- hydrochloric acid was added to dissolve the lanthanum ligature particles. Hydrochloric acid was added until the pH of the slurry reached 3. After the addition of hydrochloric acid, the pH was maintained at 3 for 1 hour, the slurry was allowed to stand, and the supernatant was removed.
- a polishing test for polishing the glass surface was performed, and the abrasive power of the abrasive was evaluated.
- the CeZLa element ratio (S) on the polished particle surface was determined by XPS analysis.
- the CeZLa element ratio (B) of the whole abrasive particles was determined by ICP analysis. Then, the following comparative examples were prepared for the present embodiment and examined similarly.
- Ratio A raw material similar to that of the first embodiment is wet-pulverized and dried, subjected to a pretreatment, and then roasted under the same conditions to obtain a roasted product (complex cerium and lanthanum).
- a roasted product complex cerium and lanthanum
- This comparative example is for confirming the generation of lanthanum ligated particles by wet pulverization.
- polishing test pure water is added to the abrasive, and the glass is polished as an abrasive slurry having a slurry concentration of 10% by weight.
- the surface of 65 mm ⁇ flat panel glass (BK-7) was polished with a polishing pad made of polyurethane using a high-speed polishing tester.
- the solid content of the abrasive slurry used was 10% by weight. Polishing was performed while supplying this at a rate of 5 LZ.
- the pressure of the polishing pad against the polishing surface was 19.6 kPa (200 gZcm 2 ), and the rotation speed of the polishing tester was set to 100 rpm.
- this polishing test was performed for 5 minutes per glass, and 20 glasses were polished, and it was examined whether or not the polishing force decreased with the increase in the number of polishing.
- the glass material after polishing was washed with pure water and dried in a dust-free state.
- the polishing value was evaluated as a relative value, with the value at the time of the first polishing of the abrasive slurry according to the first embodiment as 100.
- the composition analysis (lanthanum, cerium analysis) on the surface of the polished particles was performed using an XPS analyzer (ESCA-K1 manufactured by Shimadzu Corporation).
- the analysis conditions were an X-ray source Mg- ⁇ ray (output: 10 kV, 2 OmA), measurement interval: 0, leV, analysis area: 0.85 mm ⁇ .
- Data processing after analysis was performed as follows.
- the CeZLa element ratio (S) of the polishing particle surface was calculated.
- the CeZLa element ratio (B) of the entire abrasive particles is determined by making each of the abrasives into a solution by alkali-melting, and quantifying the content of each element by ICP analysis using the solution.
- Comparative Example 2 in which hydrochloric acid was added to Comparative Example 1 in which wet grinding was not performed, the particle surface and the entire polished particles had the same composition.However, in Comparative Example 1, a lanthanum compound was formed on the surface. This is because, as a whole, it becomes a composite oxide (solid solution)! /, So that its composition does not change when it comes into contact with hydrochloric acid.
- the abrasives according to the first and second embodiments have a higher abrasive force than the abrasive according to Comparative Example 3, as can be seen from the results of the abrasive test. Further, the abrasives according to these embodiments have an increased abrasive force according to the value of SZB. Then, it was confirmed that the abrasives according to these embodiments were excellent in the sustaining power of the polishing force, and the reduction in the polishing force was low even when polishing 20 sheets of glass. The abrasive according to Comparative Example 3 could perform a good operation when the first glass was polished, but hard clogging occurred in the polishing pad as the number of polishings increased, and the polishing power was reduced.
- the pulverization time in the wet pulverization step after roasting was changed, and pulverization was performed until the average particle diameter D was reached. Then, add salt to the slurry after grinding.
- the acid was added until the pH became 3, and the lanthanum ligated particles were dissolved and removed.
- ⁇ I In the third embodiment, the slurry after the wet pulverization was filtered without adding hydrochloric acid.
- the abrasives according to the third embodiment and the comparative example 4 were subjected to the composition analysis and the polishing test as in the first embodiment.
- the results are shown in Table 2.
- the polishing values in the table are relative values with the polishing value of the first sheet of the first embodiment being 100.
- the pulverization time in the wet pulverization step after roasting was changed, and pulverization was performed until the average particle diameter D became 0.5 m. Then, add salt to the slurry after grinding.
- the acid was added until the pH became 3, and the lanthanum ligated particles were dissolved and removed.
- ⁇ y ⁇ S In the third embodiment, the slurry after wet grinding was filtered without adding hydrochloric acid.
- the polishing values in the table are relative values where the polishing value of the first sheet of the first embodiment is 100.
- Tables 2 and 3 show that the surface element ratio of the polished particles can be changed by adjusting the grinding time. Then, it can be confirmed that the abrasives in the third and fourth embodiments have excellent sustaining power of the abrasive force similarly to the first and second embodiments. Further, it was confirmed that the abrasives according to the third and fourth embodiments had an increased abrasive force according to the value of S / B.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
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Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2005515100A JP4540611B2 (ja) | 2003-10-31 | 2004-09-29 | セリウム系研摩材及びセリウム系研摩材の製造方法 |
TW093130830A TWI266796B (en) | 2003-10-31 | 2004-10-12 | Ceric abrasive and method of producing the ceric abrasive |
Applications Claiming Priority (2)
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JP2003-373560 | 2003-10-31 | ||
JP2003373560 | 2003-10-31 |
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WO2005042661A1 true WO2005042661A1 (ja) | 2005-05-12 |
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PCT/JP2004/014197 WO2005042661A1 (ja) | 2003-10-31 | 2004-09-29 | セリウム系研摩材及びセリウム系研摩材の製造方法 |
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JP (1) | JP4540611B2 (ja) |
KR (1) | KR100679966B1 (ja) |
CN (1) | CN100351338C (ja) |
TW (1) | TWI266796B (ja) |
WO (1) | WO2005042661A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2018152575A1 (en) | 2017-02-22 | 2018-08-30 | Cmte Development Limited | Optical acoustic sensing system and method |
Families Citing this family (1)
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JP2007231158A (ja) * | 2006-03-01 | 2007-09-13 | Mitsui Mining & Smelting Co Ltd | セリウム系研摩材 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH09183966A (ja) * | 1995-12-29 | 1997-07-15 | Seimi Chem Co Ltd | セリウム研摩材の製造方法 |
JPH10183103A (ja) * | 1996-12-25 | 1998-07-14 | Seimi Chem Co Ltd | セリウム系研磨材の製造方法 |
JP2002129146A (ja) * | 2000-10-20 | 2002-05-09 | Mitsui Mining & Smelting Co Ltd | ガラス用低フッ素酸化セリウム系研摩材及びその製造方法 |
JP2003027045A (ja) * | 2000-12-25 | 2003-01-29 | Nissan Chem Ind Ltd | 酸化セリウムゾル及び研磨剤 |
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FR2795065B1 (fr) * | 1999-06-16 | 2002-04-19 | Rhodia Chimie Sa | Sol d'un phosphate de cerium et/ou de lanthane, procede de preparation et utilisation en polissage |
JP4273921B2 (ja) * | 2002-10-28 | 2009-06-03 | 日産化学工業株式会社 | 酸化セリウム粒子及び加湿焼成による製造方法 |
JP4273920B2 (ja) * | 2002-10-28 | 2009-06-03 | 日産化学工業株式会社 | 酸化セリウム粒子及び多段階焼成による製造方法 |
-
2004
- 2004-09-29 KR KR1020057010157A patent/KR100679966B1/ko not_active IP Right Cessation
- 2004-09-29 WO PCT/JP2004/014197 patent/WO2005042661A1/ja active Application Filing
- 2004-09-29 CN CNB2004800145429A patent/CN100351338C/zh not_active Expired - Fee Related
- 2004-09-29 JP JP2005515100A patent/JP4540611B2/ja not_active Expired - Fee Related
- 2004-10-12 TW TW093130830A patent/TWI266796B/zh not_active IP Right Cessation
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH09183966A (ja) * | 1995-12-29 | 1997-07-15 | Seimi Chem Co Ltd | セリウム研摩材の製造方法 |
JPH10183103A (ja) * | 1996-12-25 | 1998-07-14 | Seimi Chem Co Ltd | セリウム系研磨材の製造方法 |
JP2002129146A (ja) * | 2000-10-20 | 2002-05-09 | Mitsui Mining & Smelting Co Ltd | ガラス用低フッ素酸化セリウム系研摩材及びその製造方法 |
JP2003027045A (ja) * | 2000-12-25 | 2003-01-29 | Nissan Chem Ind Ltd | 酸化セリウムゾル及び研磨剤 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2018152575A1 (en) | 2017-02-22 | 2018-08-30 | Cmte Development Limited | Optical acoustic sensing system and method |
Also Published As
Publication number | Publication date |
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CN1795251A (zh) | 2006-06-28 |
JP4540611B2 (ja) | 2010-09-08 |
TWI266796B (en) | 2006-11-21 |
JPWO2005042661A1 (ja) | 2007-06-21 |
KR100679966B1 (ko) | 2007-02-08 |
TW200521216A (en) | 2005-07-01 |
CN100351338C (zh) | 2007-11-28 |
KR20060009230A (ko) | 2006-01-31 |
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